Technical Field
[0001]
The present invention relates to a coated a-sulfofatty acid alkyl ester salt particle
10 group, a method for producing the same, and a powder detergent.
15
Priority is claimed on Japanese Patent App1ication No. 2014-203126, filed on
October I, 2014, the content of which is incorporated herein by reference.
Background Art
[0002]
In the related art, an a:-sulfofatty acid alkyl ester salt (u-SF salt) is widely ust:d
as a surfactant formulated with a powder detergent for clothes.
In the recent years, the a:-SF salt has been manufactured as a group of particles
(a-SF salt particle group) containing the a-SF salt at a high concentration, and by
20 performing dry blending of the particle group and other detergent components, a powder
detergent has been manufactured. Therefore, until being used by being blended with the
detergent components after manufacturing, the a:-SF salt particle group is transported or
stored for a long period oftime in some cases.
If the a.-SF salt particle group is weighted down during transportation or slorl!<.l
5
2
in a high-temperature environment, unfortunately, the particles are aggregated with each
other and solidified. Particularly, if the a-SF salt particle group contains a large amowtt
of fine powder, the solidification more easily occurs.
[0003]
Regarding the aforementioned problems, PTL I discloses that. by coating th~
a-SF salt particles with a coating agent and a liquid raw material, the solidification of the
particle group containing the particles can be inhibited.
Citation List
10 Patent Literature
(0004]
[PTL 1] Japanese Unexamined Patent Application, First Publication No.
2011-116807
15 Summary of Invention
Technical Problem
[0005]
However, the technique of PTL I still needs to be ameliorated in terms of the
solidification inhibitory properties. Particularly, in a case where the a.-SF salt particle
20 group contains a large amount of fine powder, the solidification inhibitory properties are
insufficient.
[0006]
The present invention has been made in consideration of the above
circumstances, and an object thereof is to provide a coated a-sulfolatty acid alkyl ester
5
3
salt particle group having excellent solidification inhibitory properties.
Solution to Problem
[0007]
As a result of conducting intensive investigation, the inventors of the present
invention found that a coated a-sulfofatty acid alkyl ester salt particle group describe
below makes it possible to achieve the aforementioned object.
That is, the present invention has the following constitution.
[1] A coated a-sulfofatty acid alkyl ester salt particle group containing an
10 a-sulfofatty acid alkyl ester salt particles (A), and a zeolite particle group-containing
coating component (B) with which the particles (A) are coated, in which the zcol ite
particle group is a zeolite particle group (b 1) having a mean particle size of equal to or
greater than 0.8~-tm and less than 3.8 ~-
[2] The coated a-sulfofatty acid alkyl ester salt particle group described in [1],
15 in which a content of the fatty acid alkyl ester in the particles (A) is 0.9% to 4.0% by
mass, and a content of particles having a particle size of equal to or less than 35 5 J.lm in
the coated a-sulfofatty acid alkyl ester salt particle group is equal to or greater than 20%
by mass.
[3] The coated a-sulfofatty acid alkyl ester salt particle group described in 111 or
20 [2], in which when the particles (A) are thermally analyzed using a differential scanning
calorimeter, an observed heat absorption peak area S l at a temperature of 50°C to 130°C
is less than 50% of a heat absorption peak area S2 at a temperature of0°C to 130°C.
[4] A powder detergent containing the coated a-sulfofatty acid alkyl ester salt
particle group described in any one of [ 1] to [3].
4
[5] A method for manufacturing the coated a-sulfofatty acid alkyl ester salt
particle group described in any one of [1] to [3], including a step of coating the
a-sulfofatty acid alkyl ester salt particles (A) with the zeolite particle group-containing
coating component (B), in which the zeolite particle group is the zeolite particle group
5 (bl) having a mean particle size of equal to or greater than 0.8 J.lffi and less than 3.8J.lm.
[6] The method for manufacturing the coated a-sulfol'atty acid alkyl ester salt
particle group described in {5]. in which the content ofthe particles having a particle size
of equal to or less than 355 J.lm in the particle group constituted with the particles (A) is
equal to or greater than 20% by mass, and the content of the fatty acid alkyl ester in the
10 particles (A) is 0.9% to 4.0% by mass.
[71 The method for manufacturing the coated a-sulfofatty acid alkyl ester salt
particle group described in {5] or {6], further including a particle (A) manufacturing step
of manufacturing the particles (A), in which the particle (A) manufacturing step includes
a sulfonation treatment for causing sulfonation by bringing the fatty acid alkyl ester into
15 contact with a sulfonation gas, and a molar ratio of the sulfonation gas to the fatty aL:io
alkyl ester in the sulfonation treatment is 1.05 to 1.13.
{0008]
[8] A coated a-sulfofatty acid aJkyl ester saJt particle group containing
a-sulfofatty acid alkyl ester saJt particles (A) and a zeolite particle group-containing
20 coating component (B) with which the particles (A) are coated, in which the coating
component (B) contains at least one kind (b2) selected from a fatty acid alkyl ester, a
higher alcohol having 8 to 22 carbon atoms, and polyethylene g.ly\..'ol.
[9] The coated a-sulfofatty acid alkyl ester salt particle group described in [8],
in which the coating component (B) further contains a zeolite particle group (b I) having
5
a mean particle size of equal to or greater than 0.8 ~m and less than 3.8 ~·
[l OJ The coated a~sulfofatty acid alkyl ester salt particle group described in [8]
or [9], in which when the particles (A) are thermally analyzed using n difkr~fllial
scanning calorimeter, an observed heat absorption peak areaS 1 at a temperature of sooc
5 to 130°C is less than 50% of a heat absorption peak area S2 at a temperature of ooc to
130°C.
[ll] A powder detergent containing the coated a~sulfofatty acid alkyl ester salt
particle group described in any one of[8] to [10].
[12] A method for manufacturing the coated a-sulfofatty acid alkyl ester salt
10 particle group described in any one of[8] to [10}, including a step of coating the
a.-sulfofatty acid alkyl ester salt particles (A) with the zeolite particle group-containing
coating component (B), in which the coating component (B) contains at least one kind
(b2) selected from a fatty acid alkyl ester, a higher alcohol having 8 to 22 carbon atoms.
and polyethylene glycoL
15 [13] The method for manufacturing the coated a:~sulfofatty acid alkyl ester salt
particle group described in [11] or [12], further including a particle (A) manufacturing
step of manufacturing the particles (A), in which the particle (A) manufacturing step
includes a sulfonation treatment for causing sulfonation by bringing the fatty acid alkyl
ester into contact with a sulfonation gas, and a molar ratio ofth~ sulfonation gHs tu th~
20 fatty acid alkyl ester in the sulfonation treatment is 1.05 to 1.13.
[0009]
[14] a-sulfofatty acid alkyl ester salt-containing powder containing a-sulfofatty
acid alkyl ester salt particles (A), in which a content of particles having a particle size of
equal to or less than 355 ).J.m is equal to or greater than 20% by mass, and a content of the
5
6
fatty acid alkyl ester in the particles (A) is 0.9% to 4.0% by mass.
[15] The a-sulfofatty acid alkyl ester salt-containing powder described in [14],
in which the particles (A) are coated with a zeolite particle group-containing coating
component (B).
[16] The a-sulfofatty acid alkyl ester salt-containing powder described in [15],
in which the zeolite particle group contains a zeolite particle group (b3) having a mean
particle size of equal to or greater than 3.8 ~m and equal to or less than 5.0 ~1111
[17] The a-sulfofatty acid alkyl ester salt-containing powder described in any
one of [14] to [16], in which when the particles (A) are thennally analyzed using a
1 0 differential scanning calorimeter, an observed heat absorption peak area S 1 at a
15
temperature of 50°C to 130°C is less than 50% of a heat absorption peak area S2 at a
temperature of0°C to 130°C.
[18] A powder detergent containing the a-sulfofatty acid alkyl ester
salt-containing powder described in any one of[14] to [17].
[19] A method for manufacturing the a-sulfofatty acid alkyl ester salt-containing
powder described in any one of [14] to [ 17], including a particle (A) manufacturing step
of manufacturing a-sulfofatty acid alkyl ester salt particles (A), in which the particle (A)
manufacturing step includes a sulfonation treatment for causing sulfonation by bringing
the fatty acid alkyl ester into contact with a sulfonation gas, and a molar ratio of the
20 sulfonation gas to the fatty acid alkyl ester in the sulfonation treatment is 1.05 to 1.13.
[20] The method for manufacturing the a-sulfofatty acid alkyl ester
salt-containing powder described in [19], further including a step of coating the particles
(A) with a zeolite particle group-containing coating comron~.:nt ( B l.
[21] The method for manufacturing the a-sultofatty acid alkyl estt:r
7
salt-containing powder described in [20], in which the zeolite particle group contains a
zeolite particle group (b3) having a mean particle size of equal to or greater than 3.8 J..Ul1
and equal to or less than 5.0 j.tm.
5 Advantageous Effects of Invention
[0010]
The coated a-sulfofatty acid alkyl ester salt particle group of the present
invention has excellent solidification inhibitory properties.
10 Description of Embodiments
[0011]

The coated a-sulfofatty acid alkyl ester salt particle group (hereinafter, referred
to as a "coated l:l-SF salt particle group" as well) of the present invention is a group of
15 coated a-sulfofatty acid alkyl ester salt particles in which a-sulfofatty acid alkyl ester
salt particles (A) are coated with a zeolite particle group-containing coating component
(B).
20
[0012]
(First embodiment)
In a coated a-SF saJt particle group according to a first embodiment of the
present invention, a-sulfofatty acid alkyl ester salt particles (A) are coated with a coating
component (B) containing a zeolite particle group (b I) having a mean particle size of
equal to or greater than 0.8 J.lm and less than 3.8 11m.
[0013]
8
The mean particle size of the coated a-SF salt particle group is preferably 250
!-lm to 3 mm, and more preferably 350 !liD to 1 mm. If the mean particle size of the
particle group is equal to or greater than 250 /-LID, solidification is more easily inhibited.
If the mean particle size of the particle group is equal to or less than 3 mm, when the
5 coated a-SF salt particle group is formulated with a powder detergent or the like, an
extremely big difference does not easily occur between the coated a-SF salt particle
group and other components, and hence the problem of separation or the like can be
easily prevented.
The mean particle size of the coated a-SF sah particlt: group or th~ pn.::--~!ll
I 0 invention is a value measured as below.
[0014]
By using 9 stages of sieves with apertures having sizes of 1, 700 ~m. 1, 400 J.un,
1,180 J..Lrn, 1,000 !-lm, 710 ~m. 500 J..Lm, 355 J..tm, 250 ~m. and 150 J.tm, and a saucer, a
particle classification operation is perfonned. For the classification operation, the
15 sieves are piled up on the saucer in order from a sieve with small apertures to a sieve
with large apertures. The particles are put into the sieves from above tl1c I. 700 f.tlll
sieve in the uppermost portion in an amount of 100 g each time, and the sieve is capped.
The sieves are mounted on a Ro-Tap type sieve shaker (manufactured by DALTON
CORPORATION, tapping: 125 times/min. rolling: 250 times/min) and shaken for 3.5
20 minutes, and then the samples remaining on each sieve and the saucer are collected for
each sieve aperture. By repeating the aforementioned operation, classified samples are
obtained which have particles sizes of greater than 1,400 11m and equal to or less than
1, 700 ~rn ( l ,400 Jlrn. on), greater than 1,180 Jlm and equal to or less than I ,400 11m
(1,180 J..Lm. on), greater than 1,000 J..Lrn and equal to or less than 1, 180J.tm (I ,000 ).l.m. on),
9
greater than 710 J.Lffi and equal to or less than 1,000 J.1ffi (710 J.Lffi. on), greater than 500
J.Ul1 and equal to or less than 710 J.Lrn (500 J.Lrn. on), greater than 355 j.lffi and equal to or
Jess than 500 J..lffi (355 IJ.ffi. on), greater than 250 J.1ffi and equal to or less than 355 J..lm
(250 J..Lm. on), greater than 150 f.lill and equal to or less than 250 J..lffi (150 J..lffi. on), and
5 the size of particles on the saucer and equal to or less than 150 11m (150 J..lffi. pass), and a
mass frequency (%) is calculated.
The aperture ofthe sieve is denoted by X, and the sum of~ass frequencies(%)
of the classified samples collected onto the sieves having the aperture X Wid the aperture
greater than X is denoted by Y
10 The slope of a least square approximation line at the time of plotting
log{log(lOO/Y)} with respect to logX is denoted by a, and an intercept is denoted by y
(log is a common logarithm). Here, the points at which Y is equal to or less than 5%
and equal to or greater than 95% are excluded from the aforementioned plot.
By using a andy described above, a mean particle size can be detem1incd by the
15 following equation.
Mean particle size (mass 50% diameter)= to«·05Zi -y)la)
[0015]
The bulk density of the coated a-SF salt particle group is preferably 0.55 to 0.75
kg/L, and more preferably 0.60 to 0. 70 kg/L. If the bulk density of the particle group is
20 within the above preferred range, the solubility can be easily improved, and space can be
saved at the time of storage. The bulk density is measured based on JIS K33 62: 1998.
[0016]

The component (A) is a-sulfofatty acid alkyl ester salt particles.
10
The component (A) is particles containing an a-sulfofatty acid alkyl ester salt
(a.-SF salt) at a high concentration. The particles contain the a-SF salt in an amount of
equal to or greater than 60% by mass.
The content of the a-SF salt in the component (A) is preferably equal to or
5 greater than 70% by mass, and more preferably equal to or greater than 80% by mass.
10
[0017}
The a-SF salt contained in the component (A) is represented by the following
Formula (1).
R1-CH(S03M)--COOR2
.•• (1)
[In Formula (1), R1 is a linear or branched alkyl group having 6 to 20 carbon
atoms or a linear or branched alkenyl group having 6 to 20 carbon atoms, R2 is an alkyl
group having 1 to 6 carbon atoms, and M is a counter ion.]
[0018]
The number of carbon atoms of R 1 is preferably 8 to 18, and more preferably 12
15 to 16.
20
The number of carbon atoms ofR2 is preferably 1 to 3. Examples ofR2
include a methyl group, an ethyl group, a propyl group, and an isopropyl group. R 2 is
preferably a methyl group, an ethyl group, or a propyl group because these funller
improve detergency.
Examples ofM include an alkali metal slat such as sodium or potassium, an
amine salt such as rnonoethanolamine, diethanolamine, or triethanolamine, an
ammonium salt, and the like. Among these, an alkali metal salt is preferable, and a
sodium salt or a potassium salt is more preferable.
It is preferable that, in the a-SF salt, R 1 consists of 14 carbon atoms and 16
5
11
carbon atoms at a mass ratio of 40:60 to 100:0. Furthermore, the a-SF salt is preferably
an a-sulfofatty acid methyl ester salt (MES salt) in which R2 is a methyl group.
One kind of the a-SF sa1t may be used singly, or two or more kinds thereof may
be used in combination.
[0019]
The component (A) may contain, in addition to the a-SF sa1t, a by-product such
as an a-sulfofatty acid metal salt or an alkyl sulfate metal salt or moisture that is
adjunctively produced in the synthesis process of the a-SF sa1t. Generally, the
component (A) contains the a-SF salt in an amount of 60% to 98% by mass, an
10 a-sulfofatty acid metal salt in an amount of 1% to 10% by mass, and an alkyl sulfate
metal sa1t in an amount of 1% to 10% by mass.
The amount of moisture in the component (A) is preferably equal to or less than
10% by mass, and more preferably equal to or less than 5% by mass. Ifthe amount of
moisture in the component (A) is equal to or less than 10% by mass, the stickiness ofthe
15 component (A) at a low temperature can be easily suppressed, and the storage stability at
a low temperature can be easily improved.
[0020]
The component (A) preferably contains a fatty acid alkyl ester. Examples of
the fatty acid alkyl ester include a compound represented by the following Fonnula (2).
20 R3COOR4
... (2)
[In Formula (2), R3 is a linear or branched alkyl group having 7 to 2 I carbon
atoms or a linear or branched alkenyl group having 7 to 21 carbon atoms, and R~ is an
alkyl group having 1 to 6 carbon atoms.]
[0021]
12
The number of carbon atoms ofR3 is preferably 9 to 19, and more preferably 13
to 17.
The number of carbon atoms of R4 is preferably 1 to 3. Examples of R-l
include a methyl group, an ethyl group, a propyl group, and an isopropyl group. The
5 fatty acid alkyl ester is particularly preferably a fatty acid methyl ester (ME) in which R4
is a methyl group.
It is preferable that, in the fatty acid alkyl ester, R3 consists of 15 carbon atoms
and 17 carbon atoms at a mass ratio of 40:60 to 100:0.
One kind of the fatty acid alkyl ester may be used singly, or two or more kinds
10 thereof may be used in combination.
15
The aforementioned fatty acid alkyl ester may be the same as or different from
the fatty acid alkyl ester which is a raw material at the time of manufacturing the a-SF
salt.
[0022]
The content of the fatty acid alkyl ester in the component (A) is, with respect to
the total mass of the component (A), preferably equal to or greater than 0.9% by mass,
more preferably equal to or greater than 1.0% by mass, and even more preferably equal
to or greater than 1.5% by mass. If the content of the fatty acid alkyl ester in the
component (A) is the preferred amount described above, a coated a-SF salt particle
20 group having excellent solidification inhibitory properties is easily obtained.
The content of the fatty acid alkyl ester in the component (A) is, with respect to
the total mass ofthe component (A), preferably equal to or less than 4.0% by mass, more
preferably equal to or less than 3.5% by mass, and even more preferably equal to or less
than 2.5% by mass. If the content of the fatty acid alkyl ester in the component (A) is
25 the preferred amount described above, it is easy to obtain a coated a-SF salt particle
13
group with a high content of an a.-SF salt which is an active component.
The content of the fatty acid alkyl ester in the component (A) is, with respect to
the total mass of the component (A), preferably 0.9% to 4.0% by mass, more preferably
1.0% to 3.5% by mass, even more preferably 1.5% to 3.5% by mass, and particularly
5 preferably 1.5% to 2.5% by mass. If the content ofthe fatty acid alkyl ester in the
component (A) is within the preferred range described above, it is easy to obtain a coated
a.-SF salt particle group having excellent solidification inhibitory properties with a high
content of an active component.
Regarding the aforementioned fatty acid alkyl ester, for example, at the time of
I 0 manufacturing the aforementioned a.-SF salt, a reaction molar ratio between the fatty
acid alkyl ester as a raw material and a sulfonation gas may be adjusted such that the
unreacted fatty acid alkyl ester is contained in the component (A) within the
aforementioned range. Alternatively, after the a-SF salt is manufactured, the fatty acid
alkyl ester may be added such that the fatty acid alkyl ester is contained in the component
15 (A) within the aforementioned range. It is preferable to use the former method because
then the number of manufacturing steps is reduced, and the productivity becomes
excellent.
[0023}
The mean particle size of the group of the component (A) is preferably 250 to
20 3,000 IJ.ffi, and more preferably 350 to 1,000 1-1m. If the mean particle size ofthe group
of the component (A) is equal to or greater than 250 J.Lffi, the solidification of the coated
a-SF salt particle group of the present invention is more easily inhibited. Ifthe mean
particle size of the group of the component (A) is equal to or less than 3,000 J-Lm, when
the coated a-SF salt particle group of the present invention is formulated with a powder
14
detergent or the like, an extremely big difference does not easily occur between the
coated a-SF salt particle group and other components, and hence the problem of
separation or the like can be easily prevented.
The mean particle size of the group ofthe component (A) is a value determined
5 by the same method as used for determining the mean particle size of the coated ex-SF
salt particle group.
[0024]
The group of the component (A) may contain particles having a particle size of
equal to or less than 355 ~m (hereinafter, referred to as "fine powder" as well), in an
1 0 amount of equal to or greater than 20% by mass with respect to the total mass of the
group of the component (A). If the content ofthe fine powder in the group ofthe
component (A) is within the above range, in a method for manufacturing the component
(A) that will be described later, the classification operation can be skipped, and the
productivity is improved. In view of further improving the productivity, the content of
15 the tine powder of the group of the component (A) is preferably equal to or greater than
30% by mass with respect to the total mass of the group of the component (A). The
content of the fine powder of the group of the component (A), with respect to the total
mass of the group of the component (A), may be 100% by mass, preferably equal to or
less than 70% by mass, more preferably equal to or less than 60% by mass, and even
20 more preferably equal to or less than 50% by mass. If the content of the fine powder in
the group of the component (A) is equal to or less than the aforementioned upper limit. II
is easy to obtain a coated a-SF salt particle group having excellent solidification
inhibitory properties.
The content of the fine powder in the group ofthe component (A) is, with
15
respect to the total mass of the group of the component (A), preferably 20% to 70% by
mass, more preferably 30% to 70% by mass, even more preferably 30% to 60% by mass,
and particularly preferably 30% to 50% by mass. lfthe content of the tine powder in
the group of the component (A) is within the aforementioned preferred range, it is easy to
5 obtain a coated a.-SF salt particle group having excellent solidification inhibitory
properties, and the productivity is improved.
[0025]
The content of particles having a particle size of greater than 250 ).l1ll and equal
to or less than 355 ~min the aforementioned fine powder is preferably 20% to 50% by
10 mass with respect to the total mass of the fine powder. The content of particles having a
particle size of greater than 1 SO ~--tm and equal to or less than 250 ~--tm in the
aforementioned fine powder is preferably 20% to 50% by mass with respect to the total
mass of the fine powder. The content of particles having a particle size of equal to or
less than 150 ~min the aforementioned fine powder is 15% to 45% by mass with respect
15 to the total mass of the fine powder.
[0026]
The particle size distribution ofthe group of the component (A) is not
particularly limited. For example, the group of the component (A) has a particle size
distribution in which the content of particles having a particle size of greater than I, 180
20 ~m is 0% to 5% by mass with respect to the total mass of the group of the component (A),
the content of particles having a particle size of greater than 710 J..Lffi and equal to or less
than 1,180 Jll11 is 15% to 35% by mass with respect to the total mass of the group o!'th~
component (A), the content of particles having a particle size of greater than 355 ~--tm and
equal to or less than 710 J.lm is 15% to 55% by mass with respect to the total mass of the
16
group of the component (A), and the content of fine powder is 20% to 70% by mass with
respect to the total mass of the group of the component (A).
[0027]
As the component (A), the particles are preferable in which the content of the
5 fatty acid alkyl ester in the component (A) is 0.9% to 4.0% by mass, and the content of
fine powder in the group of the component (A) is equal to or greater than 20% by mass.
If such a component (A) is used, the productivity becomes excellent, and it is easy to
obtain a coated a.-SF salt particle group having excellent solidification inhibitory
properties.
10
15
[0028]
The component (A) can be manufactured by a known method. Alternatively, a
commerciaJiy available product can be used as the component (A).
[0029]
[Method for manufacturing component (A)]
Examples of the method for manufacturing the component (A) (particles (A))
include a method having a step of preparing a a.-SF salt-containing paste (paste preparing
step), a step of preparing flakes from the paste (flaking step), a step of preparing noodles
from the flakes (noodle preparing step), a step of preparing pellets from the noodles
(pelletizing step), and a step of obtaining particles by grinding the flakes, the noodles, or
20 the pellets (grinding step).
The (noodle preparing step) and the (pelletizing step) are optional steps and may
be skipped. Furthermore, after the (grinding step), a step of classifying the group of
a.·SF salt particles (classifying step) may be perfonned. In addition, after the (!laking
step), the (noodle preparing step), or the (pelletizing step), a step of maturing the flakes,
25 the noodles. or the pellets (maturing step) may be performed.
17
[0030]
[Paste preparing step]
In the paste preparing step, for example, by performing a sulfonation treatment
for causing sulfonation by bringing the fatty acid alkyl ester as a raw material into
5 contact with a sulfonation gas (S03) or the like, an esterification treatment for causing
esterification by adding a lower alcohol having 1 to 6 carbon atoms to the sulfonated
substance obtained by the sulfonation treatment, a neutralization treatment for
neutralizing the esterified substance obtained by the esterification treatment, and a
bleaching treatment for bleaching the neutralized substance obtained by the
10 neutralization treatment, an a-SF salt-containing paste are obtained. The a-SF
salt-containing paste obtained in this way generally contains, in addition to the a-SF salt,
a by-product such as a-sulfofatty acid metal salt or alkyl sulfate metal salt, methanol,
water, a fatty acid alkyl ester which is an unreacted raw material, and the like. The
aforementioned bleaching treatment may be skipped_
15 The a-SF saJt-containing paste may also be prepared in a manner in which the
a-SF salt-containing paste obtained as above is cooled and then solidified, the solidified
resultant is stored in a silo, a flexible container bag, or the like, and then the resultant is
melted again so as to be restored into a paste. Furthermore, the a-SF salt-containing
paste may be prepared by heating and melting a commercially available a-SF salt as it is
20 or by adding an appropriate amount of water thereto.
[0031]
In the aforementioned sulfonation treatment, a molar ratio of the sulfonation gas
to the fatty acid alkyl ester as a raw material (molar ratio represented by "sulfonation
gas/fatty acid alkyl ester") is preferably 1.05 to 1.13, more preferably 1.07 to 1.11, and
18
even more preferably 1.07 to 1.10. If the molar ratio ofsulfonation gas/fatty acid alkyl
ester is within the above range, the content of the fatty acid ester in the component (A) is
easily adjusted to be within the aforementioned desired preferred range. Furthermore, it
is easy to inhibit the lengthening of the time required for the sulfonation treatment and to
5 inhibit the decrease in yield of the a·SF salt.
[0032]
[Flaking treatment]
During the flaking treatment, at the time of making the a-SF salt-containing
paste into solids by cooling, the paste is made into flat plate-like solids by using a flaker,
10 a belt cooler, or the like, and then the flat plate-like solids are disintegrated using a
disintegrator, thereby obtaining a.-SF salt-containing flakes. At the time of making the
a-SF salt-containing paste into solids by cooling, if necessary, the paste may be
concentrated using a vacuum thin-film evaporator or the like.
Examples of the aforementioned flaker include a drum flaker manufactured by
15 KATSURAGI IND. CO., LTD., a drum flaker FL manufactured by Mitsubishi Materials
Corporation, and the 1ike. Examples of the belt cooler include a double belt cooler or an
NR-type double belt cooler manufactured by Nippon Belting Co., Ltd., a double belt
cooling system manufactured by Sandvik, and the like. Examples of the disintegrator
include a flake crusher FC manufactured by Hosokawa Micron Group, and the like.
20 [0033]
[Noodle preparing step]
During the noodle preparing step, the a.-SF salt-containing flakes are melted, put
into an extrusion granulator or a kneader, and pass through a dice having an appropriate
diameter, thereby obtaining noodles.
19
Examples of the extrusion granulator include PELLETER DOUBLE and TWIN
DOME GRAN manufactured by Fuji Paudal co., ltd, a gear pelletizer and Extrud-0-Mix
manufactured by Hosokawa Micron Group, and the like.
The aforementioned kneader is not particularly limited, and examples thereof
S include a continuous or batch-type kneader. The kneader also includes kneaders having
a blade or the like which is for forcedly stirring and mixing the contents in the device.
Examples of the continuous kneader include a KRC kneader, a KEX extruder,
and an SC processor manufactured by KURIMOTO, LTD., Extrud-0-Mix manufactured
by Hosokawa Micron Group, a twin-screw/single~screw extruder and FEEDER RUDER
10 manufactured by MORIYAMA, and the like. Examples ofthe batch-type kneader
include a batch kneader/pressurizing kneader manufactured by KURIMOTO. LTD., a
universal mixing and stirring machine manufactured by DALTON CORPORATION, a
general mixer and a pressurizing kneader manufactured by MORIYAMA. a NAUTA
MIXER manufactured by Hosokawa Micron Group, a Lodige mixer manufactured by
15 MATS UBO Corporation, a pro~ shear mixer manufactured by Pacific Machinery &
Engineering Co., Ltd, and the like. In view of smoothly moving the kneaded substance
to the next step, it is preferable to use the continuous kneader.
20
25
[0034]
[Pelletizing step]
During the pelletizing step, the a-SF salt-containing noodles are disintegrated in
an arbitrary size by using a disintegrator or the like, thereby obtaining a-SF
salt-containing pellets. Examples ofthe disintegrator include NIBBLER manufactured
by Hosokawa Micron Group, and the like.
[0035]
[Grinding step]
20
During the grinding step, the aforementioned flakes, pellets, or noodles are
ground by a grinder, thereby obtaining the component (A). Examples of the grinder
include a hammer mill, a pin mill, and the like. Examples of the hammer mill include a
feather mill FS manufactured by Hosokawa Micron Group, a Fitzmill manufactured by
5 FitzPatrick Company, and the I ike.
[0036]
The internal temperature of the grinder at the time of grinding is not particularly
limited, but is preferably 30°C to 50°C, more preferably 30°C to 40°C, and even more
preferably 33°C to 38°C. If the internal temperature is equal to or higher than 30°C, the
10 particle size distribution ofthe obtained particles is easily narrowed. and the occurrence
of fine powder is easily inhibited. If the internal temperature is equal to or lower than
50°C, the stickiness of the particles can be easily reduced, and it is easy to inhibit the
partic1es from adhering to the device. Therefore, the productivity is easily improved.
At the time of grinding, it is preferable to mount a screen on the grinder. For
15 example, in a case where the amount of coarse powder is expected to increase, a screen
with holes having a diameter of2 rnm is used, and in a case where the amount of fine
powder is expected to increase, a screen with holes having a diameter of 3 to 5 mm is
used.
The rotation frequency of the disintegration blade at the time of grinding is
20 preferably 200 to 8,000 rpm, and more preferably 600 to 5,000 rpm. The higher the
rotation frequency is, the easier it is for the particle size of the obtained particles to be
small. and the lower the rotation frequency is, the easier it is for the particle size to be
large. The circumferential speed of the tip of the disintegration blade is preferably 20 to
70 m/s, more preferably 30 to 60 rnls, and even more preferably 35 to 55 m/s. The
25 grinding time is generally 5 seconds to 5 minutes. Multiple grinders may be arranged in
series or in a row.
[0037]
[Classifying step]
21
During the classifying step, by using a classifying device, the particle size ofthe
5 group of the component (A) is adjusted to be within a desired range. The classifying
device is not particularly limited, and known classifYing devices can be used. However,
it is preferable to use sieves. Among the sieves, a gyro-type sieve, a flat sieve, and a
shaking sieve are preferable. The gyro-type sieve is a sieve obtained by making a flat
sieve, which slightly slants, performs horizontal circular motion. The flat sieve is a
10 sieve obtained by making a flat sieve, which slightly slants, perfonns a reciprocating
motion practically in parallel to the plane. The shaking sieve is a sieve that rapidly
shakes in a direction which is practically perpendicular to the plane of the sieve. It is
preferable that the sieving is performed for equal to or longer than 5 seconds. In order
to improve the efficiency of sieving, tapping balls can be used.
15 [0038]
Generally, the group of the component (A) before the classifying step contains
fine powder in an amount of equal to or greater than 30% by mass, although the amount
varies with the manufacturing conditions or the like.
If the content of the fine powder in the group of the component (A) is great,
20 solidification easily proceeds during storage. Accordingly, for inhibiting the
25
solidification, the amount ofthe fine powder in the group of the component (A) is
adjusted by performing the classifying step, such that the content of the fine powder in
the group of the component (A) is adjusted and becomes, for example, less than 20% by
mass.
However, in the present invention, by coating the component (A) with the
22
component (B), the solidification inhibitory properties are improved. Therefore, even
when the amount of the fine powder in the group of the component (A) is equal to or
greater than 20% by mass, it is possible to obtain a coated a-SF salt particle group
having excellent solidification inhibitory properties. Furthermore, if the content of the
5 fatty acid alkyl ester in the component (A) is 0.9% to 4.0% by mass, the solidification
inhibitory properties are further improved.
Consequently, the content of the fine powder in the group of the component (A)
is not particularly limited. As the group of the component (A), it is preferable to use a
component in which the content of the fine powder may be 100% by mass or preferably
10 equal to or less than 70% by mass, more preferably equal to or less than 600/o by mass,
and even more preferably equal to or less than 50% by mass, because then the
aforementioned classifying operation can be skipped, and the productivity is improved.
Furthermore, as the group of the component (A), it is preferable to use a component in
which the content of the fine powder is equal to or greater than 20% by mass and more
15 preferably equal to or greater than 30% by mass, because then the solidification
inhibitory effect ofthe present invention can be more effectively obtained. Ifthe
content of the fine powder is great, the mean particle size of the particle group of the
component (A) becomes small. In a case where such particles are formulated with a
powder detergent, there may be a big difference in a particle size between the pllrticles
20 and other components, and the problem of separation may occur. In this respect, the
content of the fine powder in the group of the component (A) is preferably equal to or
less than 50% by mass.
[0039]
The content of the fine powder in the group of the component (A) is preferably
25 20% to 70% by mass, more preferably 30% to 70% by mass, even more preferably 30%
23
to 60% by mass, and particularly preferably 30% to 50% by mass.
[0040]
As the component (A), a component is preferable in which the content of the
fatty acid alkyl ester in the component (A) is 0.9% to 4.0% by mass, and the content of
5 the fine powder in the group of the component (A) is equal to or greater than 20% by
mass. If the aforementioned component (A) is used, the productivity becomes excellent,
and it is easy to obtain a coated a-SF salt particle group having excellent solidification
inhibitory properties.
10
[0041]
[Maturing step 1
It is known that, in the flakes, noodles, pellets, and particles containing the a-SF
salt (hereinafter, these will be collectively referred to as an "a-SF salt-containing solid"
as well), there are a metastable crystalline state and a stable crystalline state which is
formed by crystallizing the a-SF salt-containing solid. Furthermore, it is known that
15 the solidification inhibitory properties of the a-SF salt-containing solid in the stable
crystalline state (hereinafter, referred to as a "stable solid" as well) are better than those
of the a-SF saJt-containing solid in the metastable crystalline state (hereinafter, referred
to as a "metastable solid" as well) (see PCT International Publication No.
W02009/054406).
20 [0042]
Generally, it is difficult to form a metastable solid from an a-SF salt with high
purity. If an a-SF salt is obtained through each of the aforementioned steps by using a
fatty acid alkyl ester as a starting material, usually, in addition to the a-SF salt, a
by-product such as an alkyl sulfate metal salt or an a-sulfofatty acid salt is generated. If
24
the a-SF salt-containing solid contains such a by-product, the a-SF salt-containing solid
easily becomes in a metastable state.
[0043]
During the maturing step, the metastable solid is converted into a stable solid.
5 The method for converting the metastable solid into the stable solid is known,
10
and examples thereof include the following methods (1-1) to (1-3).
(1-1) A method of keeping the metastable solid for at least 48 hours at a
temperature of equal to or higher than 30°C under a pressure of equal to or lower than
200,000 Pa.
(1-2) A method of keeping a melt, which is obtained by melting the metastable
solid, for 5 minutes or longer at a temperature that is equal to or higher than the melting
point of the metastable solid and is equal to or lower than the melting point of the stable
solid.
(I-3) A method of applying a shearing force to a melt, which is obtained by
15 melting the metastable solid, at a shearing rate of equal to or higher than 1 00 ( 1/s) at a
temperature that is equal to or higher than the melting point of the metastable solid and is
equal to or lower than 80°C.
[0044]
The metastable solid and the stable solid can be easily differentiated from each
20 other through thermal analysis using a differential scanning calorimeter Wh~:n the:
metastable solid is thennally analyzed using a differential scanning calorimeter, an
observed heat absorption peak areaS 1 at a temperature of sooc to 130°C is less than
50% of a heat absorption peak area S2 at a temperature of ooc to 130°C. 1 n contrast.
when the stable solid is thermally analyzed using a differential scanning calorimeter, an
25
observed heat absorption peak area S 1 at a temperature of sooc to 130°C is equal to or
greater than 50% of a heat absorption peak area S2 at a temperature of ooc to 130°C.
[0045]
In the present invention, by coating the component (A) with the component (B),
5 the solidification inhibitory properties are further improved. Therefore, even if the
component (A) is the metastable solid, the solidification inhibitory properties are
improved.
Accordingly, as the component (A), either the metastable solid or the stable solid
may be used. It is preferable to use the metastable solid as the component (A), because
10 then the maturing step can be skipped, and the productivity is improved.
15
Whether the component (A) is the metastable solid or the stable solid can be
easily determined by performing X-ray diffractometry or microscopic observation on
both of the solids, in addition to performing the aforementioned differential scanning
calorimetry (see PCT International Publication No. W02009/054406).
[0046]
The content of the component (A) in the coated a-sulfofatty acid alkyl ester salt
particles (hereinafter, referred to as "coated a-SF salt particles" as well) coated with the
component (B) is, with respect to the total mass of the coated a-SF salt particles,
preferably 70% to 99% by mass, more preferably 80% to 97% by mass, and even more
20 preferably 85% to 90% by mass. Ifthe content of the component (A) is equal to or
greater than 70% by mass with respect to the total mass of the coated a-SF salt particks,
the solubility of the coated a-SF salt particles is easily improved. If the content of the
component (A) is equal to or less than 99% by mass with respect to the total mass of the
coated a-SF salt particles, the solidification inhibitory effect is easily obtained.
[0047]

26
The component (B) of the present embodiment is a coating component
containing a zeolite particle group (component (bl)) having a mean particle size of equal
5 to or greater than 0.8 1-1m and less than 3.8 Jlm as a zeolite particle group.
The component (B) may contain at least one kind (component (b2)) selected
from a fatty acid alkyl ester, a higher alcohol having 8 to 22 carbon atoms, and
polyethylene glycol.
The component (B) may contain optional components other than the component
10 (b 1) and the component (b2), within a range that does not impair the effect of the present
invention.
ln view of improving the solidification inhibitory properties, the component (B)
preferably consists of the component (bl). In view of inhibiting the generation of dust
at the time of manufacturing the coated a-SF salt particle group of the present invention,
15 in view of improving the solidification inhibitory properties of the coated a-SF salt
particle group containing a large amount of fine powder, and in view of improving the
solidification inhibitory properties in a case where the component (A) is the metastable
solid, the component (B) preferably consists of the component (bl) and the component
(b2).
20 [0048}
The content of the component (B) in the coated a-SF salt particles is, with
respect to the total mass of the coated a-SF salt particles, preft:rably I% to 30'Yo by mass.
more preferably 3% to 20% by mass, and even more preferably 10% to 15% by mass.
If the content ofthe component (B) is equal to or greater than I% by mass with respect to
27
the total mass of the coated a.-SF salt particles, the solidification inhibitory effect is
easily obtained. Furthermore, if the content of the component (B) is equal to or less
than 30% by mass with respect to the total mass of the coated a-SF salt particll.!s, in a
case where the coated a-SF salt particles are formulated with a powder detergent, it is
5 easy to maintain a degree of freedom in formulating the particles with other components.
[0049]
In the coated a-SF salt particles, the proportion of a surface area of the
component (A) coated with the component (B) is preferably equal to or greater than 30%,
more preferably equal to or greater than 50o/o, and even more preferably equal to or
10 greater than 70%. The proportion may be I 00%.
The ratio (coating ratio) ofthe coated area to the surface area of the component
(A} can be checked by, for example, observing the surface of the coated a-SF salt
particles by using a microscope (manufactured by ASAHI KOGAKUKI MANUF. CO.,
LTD., Handi Scope TM) or a scanning electron microscope (for example, S-2380N
15 manufactured by Hitachi, Ltd.) and an energy dispersive X-ray analyzer (for example,
EMAX-7000 manufactured by HORIBA, Ltd.) and performing image analysis, surface
element analysis, or the like.
20
[00501

The component (bl) is a zeolite particle group having a mean partidc sizl' or
equal to or greater than 0.8 )..lm and less than 3.8 ~. By coating the component (A)
with the component (bl), the solidification of the coated a-SF salt particle group ofthe
present invention can be inhibited.
[0051]
28
The mean particle size of the component (bl) is equal to or greater than 0.8 IJ.m
and less than 3.8 llffi. The mean particle size is preferably 1.0 to 3.4~-Lm. and more
preferably l.O to 3.0 j..lm. If the mean particle size ofthe component (bl) is equal to or
greater than 3.8 J.lm, the solidification inhibitory effect is not sufficiently obtained. If
5 the mean particle size of the component (bl) is less than 0.8 j..Ull, the zeolite particles are
aggregated with each other, and the solidification inhibitory effect is not sufficiently
obtained.
[0052]
The smaller the mean particle size of the component (b 1) is, the easier it is to
10 obtain an excellent solidification inhibitory effect. However, if the mean particle size is
too small, the zeolite particles are aggregated with each other, and the solidification
inhibitory effect is not sufficiently obtained. In this respect, the lower limit of the mean
particle size of the component (bl) is equa1 to or greater than 0.8 J.lffi. The lower limit is
preferably equal to or greater than 1.0 llffi, and more preferably equal to or greater than
15 2.0 J.lffi. In contrast, in view of obtaining an excellent solidification inhibitory effect.
the upper limit of the mean particle size of the component (b I) is less than 3.8 pm The
upper limit is preferably equal to or less than 3.4 )..Lnl, more preferably equal tour ks:.
than 3.0 J.lm, and even more preferably equal to or less than 2.8 j..lm.
The mean particle size of the component (bl) is a volume-based median
20 diameter measured by a device (for example, a particle size distribution analyzer (LS13
320, manufactured by Beckman Coulter, Inc.)) using a laser diffraction/scattering
method.
[0053]
As the component (bl), a natural substance or a synthetic product may be used.
29
Examples of the zeolite of the component (b 1) include A-type zeolite, P-type zeolite,
faujasite-type zeolite, and the like. Among these, the A-type zeolite is preferable.
[0054)
Examples of the zeolite particle group include the commercially availabk
5 products shown in Table l. Table 1 shows the mean particle size of the zeolite particle
group as a commercially available product that is determined by the measurement
method of the present invention.
[0055]
[Table 1]
Manufacturer of zeolite particle group
Mean partic1e size of zeolite particle group
(~m)
Guangzhou Hengbang
Fine Chemical 4.0 to 4.6
Chalco 3.8 to 4.2
Huiying Chemical 4.2
Yue Xiu Textiles 4.7
10 [0056]
The mean particle size of the zeolite particle group as a commercially available
product shown in Table 1 is greater than the upper limit of the range of the mean particle
size of the component (b 1) of the present invention. Such a zeolite particle group is
prepared by sieving, pulverizing, or the like such that the zeolite particle group has a
15 desired mean particle size, and can be used as the component (b 1) of the present
invention.
[0057]
Any one kind of the component (b I) may be used singly, or two or more kinds
thereofmay be used in combination.
20 The content ofthe component (b 1) in the component (B) is, with respect to the
total mass of the component (B), preferably 50% to 100% by mass, more preferably 80%
30
to 100% by mass, and even more preferably 90% to 100% by mass. The content may
be 100% by mass. If the content of the component (b I) in the component (B) is equal to
or greater than 50% by mass, the solidification inhibitory effect is easily obtained.
The content of the component (b l) in the coated a.-SF salt partic1es is, with
5 respect to the total mass of the coated a.-SF salt particles, preferably 1% to 30% by mass,
more preferably 3% to 20% by mass, even more preferably 5% to 15% by mass, and
particularly preferably l 0% to 15% by mass. If the content of the component (b l) in the
coated a-SF salt particles is equal to or greater than I% by mass, the solidification
inhibitory effect is easily obtained. Ifthe content ofthe component (bl) in the coated
10 a-SF salt particles is equal to or less than 30% by mass, in a case where the coated a-SF
salt particles are fonnulated with a powder detergent, it is easy to maintain a degree of
freedom in fonnulating the particles with other components.
[0058]

15 The component (b2) is at least one kind selected from a fatty acid alkyl ester, a
higher alcohol having 8 to 22 carbon atoms, and polyethylene glycol.
Because the component (B) contains the component (b2), the solidification of
the coated a.-SF salt particle group of the present invention can he further inhibited.
Furthermore, in view of making it easy to inhibit the generation of dust at the time of
20 manufacturing the coated a-SF salt particle group of the present invention, in view of
making it easy to improve the solidification inhibitory properties of the coated a-SF salt
particle group containing a large amount offine powder, and in view of making it easy to
improve the solidification inhibitory properties in a case where the component (A) is the
metastable solid, the component (B) preferably contains the component (b2).
5
31
[0059]
Examples of the aforementioned fatty acid alkyl ester include the same
compound as the compound represented by Formula (2) described above.
[0060]
Examples of the higher alcohol having 8 to 22 carbon atoms include natural
higher alcohols such as capryl alcohol, decyl alcohol, Iaury! alcohol. myristyl 11lwl1ol.
cetyl alcohol, stearyl alcohol, oleyl alcohol, 2-butyloctanol, isotridecyl alcohol,
isohexadecyl alcohol, 2-butyldecanol, 2-hexyloctanol, 2-hexyldodecanol, 2-octyldecanol,
2-hexyldecanol, 2-octadecanol, and 2-dodecylhexadecanol or synthetic higher alcohols.
10 Among the higher alcohols having 8 to 22 carbon atoms, those having 10 to 20 carbon
15
atoms are preferable, and those having 14 to 18 carbon atoms are more preferable.
As the aforementioned polyethylene glycol, those having a weight-average
molecular weight of200 to 20,000 are preferable, and those having a weight-average
molecular weight of 300 to I ,500 are more preferable.
[0061]
Among the above components (b2), a fatty acid alkyl ester, and a higher alcohol
having 8 to 22 carbon atoms are preferable, and a fatty acid methyl ester (ME) is
particularly preferable. The aforementioned fatty acid alkyl ester may be the same as or
different from the fatty acid alkyl ester which is a raw material at the time of
20 manufacturing the a-SF salt.
[0062]
Any one kind of the components (b2) may be used singly, or two or more kinds
thereof may be used in combination.
The content ofthe component (b2) in the component (B) is, with respect to the
25 total mass of the component (B), preferably 0% to 50% by mass, more preferably 0% to
32
20% by mass, and even more preferably 0% to 10% by mass. If the content of the
component (b2) in the component (B) is within the aforementioned preferred range, the
solidification inhibitory effect is easily obtained.
The content of the component (b2) in the coated a-SF salt panicles is, with
5 respect to the total mass of the coated a-SF salt particles, preferably equal to or less than
10% by mass, more preferably equal to or less than 5.0% by mass, and even more
preferably equal to or less than 3.0% by mass. If the content of the component (b2) in
the coated a-SF salt particles is equal to or less than 10% by mass, the solubility of the
coated a-SF salt particles is easily improved.
10 [0063)
In view of improving the solidification inhibitory properties of the coated a-SF
salt particle group of the present invention, the component (B) preferably consists of the
component (b1).
Furthermore, in view of inhibiting the generation of dust at the time of
15 manufacturing the coated a-SF salt particle group of the present invention, in view of
improving the solidification inhibitory properties ofthe coated a-SF salt particle group
containing a large amount of fine powder, and in view of improving the solidilication
inhibitory properties in a case where the component (A) is the metastable solid, the
component (B) preferably contains the component (b2) and more preferably consists of
20 the component (bl) and the component (b2).
In a case where the component (B) contains the component (b2), the content of
the component (bl) in the component (B) is, with respect to the total mass of the
component (B), preferably 60% to 99.8% by mass, more preferably 80% to 99.5% by
mass, and even more preferably 90% to 98% by mass. The content of the component
33
(b2) in the component (B) is, with respect to the total mass of the component (B).
preferably 0.2% to 40% by mass, more preferably 0.5% to 20% by mass, and even more
preferably 2% to 1 0% by mass.
The mass ratio of the component (b2) to the component (b1) {component
5 (b2)/component (b 1)} is preferably 0.002 to 0. 7, more preferably 0.005 to 0.25. and even
more preferably 0.02 to 0.1.
The content of the component (b I) in the coated a-SF salt particles is. with
respect to the total mass ofthe coated a-SF salt particles, preferably l% to 30% by mass,
more preferably 3% to 20% by mass, and even more preferably 10% to 15% by mass.
10 The content of the component (b2) in the coated a-SF salt particles is, with respect to the
total mass of the coated a-SF salt particles, preferably 0.1% to 10% by mass, and more
preferably 0.3% to 5% by mass.
15
[0064]

The method for manufacturing the coated a-SF salt particle group of th~ present
embodiment has a step of coating the component (A) with the component (B) (coating
step).
The method for manufacturing the coated a-SF salt particle group of the present
embodiment has, for example, a particle (A) manufacturing step of manufacturing the
20 component (A) (particles (A)), a component (B) selecting step, and a coating step of
coating the component (A) with the component (B).
[0065]
The particle (A) manufacturing step is a step of manufacturing the component
(A) by the aforementioned method for manufacturing the component tA)
34
That is, the particle (A) manufacturing step has a step of preparing an a-SF
salt-containing paste (paste preparing step), a step of preparing flakes from the paste
(flaking step), a step of preparing noodles from the flakes (noodle preparing step), a step
of preparing pellets from the noodles (pelletizing step), and a step of obtaining particles
5 by grinding the flakes, the noodles, or the pellets (grinding step).
The (noodle preparing step) and the (pelletizing step) are optionaJ steps and may
be skipped. Furthermore, after the (grinding step), a step of classifying the group of
a-SF salt particles (classifying step) may be performed. In addition, after the (flaking
step), the (noodle preparing step), and the (pelletizing step), a step of maturing the flaks,
10 the noodles, or the pellets (maturing step) may be performed.
[0066]
During the paste preparing step, for example, the following treatments an:
performed which include a sulfonation treatment for causing sulfonation by bringing a
fatty acid alkyl ester as a raw material into contact with a sulfonation gas (S0J) or the
15 like, an esterification treatment for causing esterification by adding a lower alcohol
having l to 6 carbon atoms to the sulfonated substance obtained by the sulfonation
treatment, a neutralization treatment for neutralizing the esterified substance obtained by
the esterification treatment, and a bleaching treatment for bleaching the neutralized
substance obtained by the neutralization treatment. The bleaching treatment ma~ be
20 skipped.
[0067]
As described above, in the sulfonation treatment, by adjusting the molar ratio of
sulfonation gas/fatty acid alkyl ester, the content of the fatty acid alkyl ester contained in
the component (A) can be adjusted. Furthermore, by additionally performing the
25 aforementioned classifying step, the particle size distribution of the group of the
component (A) can be adjusted.
[0068]
35
In the particle (A) manufacturing step, if the component (A) is manufactured in
which the content of the fatty acid alkyl ester in the particles (A) is 0.9% to 4.0% by
5 mass, it is easy to obtain a coated a-SF salt particle group having excellent solidification
inhibitory properties with a high content of an a-SF salt which is an active component.
Furthermore, even if either or both of the aforementioned maturing step and the
classifying step are not performed, it is easy to obtain a coated a-SF salt particle group
having excellent solidification inhibitory properties. In addition, even if the content of
10 fine powder in the group of the particles (A) is equal to or greater than 20% by mass, it is
easy to obtain a coated a-SF salt particle group having excellent solidification inhibitory
properties.
[0069)
The component (B) selecting step is a step of sel~cting a component as a zeolite
15 particle group (bl) having a mean particle size ofequaJ to or greater than 0.8 ~m and Jess
than 3.8 ~m from zeolite particle groups before the coating step.
During the selecting step, the mean particle size (volume-based median
diameter) ofthe zeolite particle group is measured by the aforementioned device using a
laser diffraction/scattering method, and whether or not the mean particle size is within a
20 desired range is checked. Then, a zeolite particle group satisfying a desired range of a
mean particle size is selected as the component (b 1) and used as a coating component for
the component (A). In a case where a zeolite particle group does not satisfy the desired
range of a mean particle size, the zeolite particle group can be subjected to sieving,
pulverizing, or the like and then subjected again to the selecting step. The selecting step
36
can be repeated (twice or more) until a zeolite particle group having a desired mean
particle size is obtained.
[0070]
In the coating step, the method for coating the component (A) with the
5 component (B) can be appropriately set according to the composition of the component
(B). Hereinafter, the coating treatment method will be described according to the
composition of the component (B).
lO
[0071]
[(Il-l): In case where component (B) consists of component (bl)]
In a case where the component (B) consists of the component (bl), examples of
the method for coating the component (A) with the component (B) include a method of
putting the component (A) and the component (B) into a mixer and mixing them
together.
Either the component (A) or the component (B) may be put first into the mixer_
15 Alternatively, both of them may be simultaneously put into the mixer.
20
The mixer is not particularly limited but is preferably a mixer used for dry
mixing. Examples thereof include a horizontal cylindrical mixer, a container
rotation-type mixer such as a V-type mixer, an agitated mixer, and the like.
[0072]
[(II-2): In case where component (B) contains component (b I) and component
(b2)]
In a case where the component (B) contains the component (bl) and the
component (b2), the coating method includes a step of coating the component (A) with
the component (b 1 ), and a step of coating the component (A) with the component (b2).
25 Either the step of coating the component (A) with the component (bl) or the step of
37
coating the component (A) with the component (b2) may be performed first.
Alternatively, both of the steps may be simultaneously performed. In view of further
improving the solidification inhibitory properties and in view of inhibiting the generation
of dust. it is preferable to perform the step of coating the component (A) with the
5 component (b2) and then perform the step of coating the component (A) with the
component (b 1 ).
Examples of the method for coating the component (A) with the component (bl)
include the aforementioned method (11-l).
Examples of the method for coating the component (A) with the component (b2)
10 include a method in which the component (A) or the component (A) coated with the
component(bl) is put into a mixer such as an agitated mixer or a contHiner rotation-typ~
mixer, the component (b2) is added thereto while the component (A) is being kept
flowing, and mixing the components together.
Examples of the method of adding the component (b2) include a method of
15 spraying the component (b2), a method of adding the component (b2) dropwise, and the
like. In view of inhibiting the generation of dust and further improving the
solidification inhibitory properties, the spra~ying method is preferable.
[0073]
Examples of the method of spraying the component (b2) include a method in
20 which the component (A) or the component (A) coated with the component (bl) is put
into a container rotation-type cylindrical mixer, and the component (b2) is sprayed from a
spray nozzle provided in the mixer while the mixer is being rotated. It is preferable that
the component (b2) is sprayed such that the component (b2) does not directly contact the
inner wall surface of the mixer. The mixer may be a batch type or a continuous type.
25 Furthermore, the number of baffles in the mixer or the shap~ lltl!r~ur is not partil.'ularl)
38
limited.
[0074]
The spray nozzle is not particularly limited, and examples thereof include a
two-fluid nozzle spraying a gas and a liquid by mixing them together, a pressurizing
5 nozzle performing spraying by applying a relatively high pressure, and the like.
10
Examples of the two-fluid nozzle include a Bl MY series and a Bl MV S series
manufactured by H. IKEUCHI Co., Ltd., and the like. Examples ofthe pressurizing
nozzle include a K series, a KB series, a VV series, a VVP series, and aVE series
manufactured by H. IKEUCHI Co., Ltd., and the like.
[0075]
At the time of spraying the component (b2), if necessary, the component (b2)
may be heated so as to obtain a desired droplet diameter. However, if the temperature
of the component (b2) is too high, in some cases, the component (b2) is excessively
atomized due to the decrease in viscosity, and hence the spray pressure increases.
15 Therefore, in order to perform spraying at a stable spray pressure, the I iqu id temperatur~
of the component (b2) is preferably room temperature (20°C) to 95°C.
[0076]

The powder detergent of the present embodiment contains the aforementioned
20 coated a-SF salt particle group.
The powder detergent of the present embodiment is easily manufactured by
mixing the coated a-SF salt particle group with other detergent CL)mron.:-nts.
Examples of the detergent components include an anionic surfactant such as a
linear alkylbenzene sulfonic acid metal salt, a. olefin sulfonic acid metal salt, an alkyl
39
sulfate metal salt, or a salt of a metallic soap; a nonionic surfactant such as an alkylene
oxide adduct of a higher alcohol or the like; an amphoteric surfactant; a cationic
surfactant; an inorganic builder such as zeolite, sodium sulfate. or sodium sulfik: ;m
alkaline agent such as sodium carbonate or potassium carbonate; a fluorescent agent; a
5 bleaching agent; a bleaching activator; an enzyme; a fragrance; a colorant; a softener; a
polymer builder such as cationized cellulose, powdered cellulose, or polysodium acrylate,
and the like.
The content of the coated a-SF salt particle group in the powder detergent is not
particularly limited, but is, with respect to the total mass of the powder detergent,
10 preferably 1% to 80% by mass, more preferably 1% to 50% by mass, and even more
preferably 5% to 40% by mass. If the content is within the above preferred range, the
solidification of the powder detergent is easily inhibited, and the fluidity is easily
improved.
The detergent with which the coated a-SF salt particle group of the present
15 embodiment is formulated is not limited to the powder detergent. The coated a-SF salt
particle group may also be formulated with, for example, a tablet-type or sheet-type solid
detergent or a liquid detergent.
20
[0077]
(Second embodiment)
In a coated a-SF salt particle group according to a second embodiment of the
present invention, a-sulfofatty acid aJkyl ester salt particles (A) are coated with a zeolite
particle group-containing coating component (B) and at least one kind (b2) selected from
a fatty acid alkyl ester, a higher alcohol having 8 to 22 carbon atoms, and polyethylene
glycol.
5
10
40
[0078]
The mean particle size of the coated a-SF salt particle group in the present
embodiment is the same as the mean particle size of the coated a-SF saJt particle group
in the first embodiment.
The bulk density of the coated a-SF salt particle group in the present
embodiment is the same as the bulk density of the coated a-SF salt particle group in the
first embodiment.
[0079]

As the component (A) in the present embodiment, it is preferable to use the
same component as the component (A} in the first embodiment.
As the group of the component (A) in the present embodiment, the same group
as the group of the component (A) in the first embodiment can be used.
[Method for manufacturing component (A)]
15 The component (A) in the present embodiment can be manufactured by the same
manufacturing method as the method for manufacturing the component (A) of the first
embodiment
[0080]
The content of the component (A) in the coated a.-SF saJt particles in the present
20 embodiment is the same as the content of the component (A) in the coated a.-SF saJt
particles of the first embodiment.
[0081]

The component (B) in the present embodiment is a coating component
5
41
containing a zeolite particle group and at least one kind (b2) selected from a fatty acid
alkyl ester, a higher alcohol having 8 to 22 carbon atoms, and polyethylene glycol.
By coating the component (A) with the coating component, it is possible to
inhibit the solidification of the coated a.-SF salt particle group of the present invention.
[0082]
The mean particle size of the aforementioned zeolite particle group is not
particularly limited. As the zeolite particle group, for example, the commercially
available zeolite particle group shown in Table 1 may be used, or the aforementioned
component (bl) may be used. As the zeolite particle group, those having a mean
10 particle size within a range of0.8 to 5.0 ~m can be preferably used. In view of
obtaining a better solidification inhibitory effect, it is preferable to use the component
(bl) as the zeolite particle group.
[0083]
As the component (bl), the same component (bl) as in the first embodiment can
15 be used.
As the component (b2), the same component (b2) as in the first embodiment can
be used.
The component (B) may contain optional components other than the zeolite
particle group and the component (b2), within a range that does not impair the effect of
20 the present invention.
[0084]
The content of the component (B) in the coated a-SF salt particles in the present
embodiment is the same as the content of the component (B) of the coated a-SF salt
particles of the first embodiment.
42
The coating ratio of the coated a-SF salt particles in the present embodiment is
the same as the coating ratio ofthe coated a-SF salt particles of the first embodiment.
[0085]
The content of the zeolite particle group in the component (B) is, with respect to
5 the totaJ mass of the component (B), preferably 60% to 99.8% by mass, more preferably
80% to 99.5% by mass, and even more preferably 90% to 98% by mass.
10
The content of the component (b2) in the component (B) is, with respect to the
tota1 mass of the component (B), preferably 0.2% to 40% by mass, more preferably 0.5%
to 20% by mass, and even more preferably 2% to I 0% by mass
In the present embodiment, because the component (B) contains the component
(b2), the generation of dust at the time of manufacturing the coated a-SF saJt particle
group is easily inhibited, the solidification inhibitory properties of the coated a-SF salt
particle group containing a large amount of fine powder are easily improved, and the
solidification inhibitory properties in a case where the component (A) is a metastable
15 solid are easily improved.
In th~;; ~;umpon,.;nt (B), tht: mass ratio of the;: ~;umpuncnt ( b2) to the zeol it~
particle group {component (b2)/zeolite particle group} is preferably 0.002 to 0 7, more
preferably 0.005 to 0.25, and even more preferably 0.02 to 0.1.
The content of the zeolite particle group in the coated a-SF salt particles is. with
20 respect to the total mass of the coated a-SF salt particles, preferably 1% to 30% by mass,
more preferably 3% to 20% by mass, and even more preferably 10% to 15% by mass.
The content of the component (b2) in the coated a-SF salt particles is, with
respect to the total mass of the coated a~SF salt particles, preferably 0.05% to I 0% by
mass, more preferably 0.1% to 5.0% by mass, and even more preferably 0.2% to 3.0% by
5
mass.
43
As the zeolite particle group, it is preferable use the component (bl).
[0086]

The method for manufacturing coated a-SF salt particles of the present
embodiment includes a step of coating the component (A) with the component ( 8)
(coating step).
The method for manufacturing a coated a-SF salt particle group of the present
embodiment includes, for example, a particle (A) manufacturing step of manufacturing
10 the component (A) (particles (A)), and a coating step of coating the component (A) with
the component (B).
[0087]
The particle (A) manufacturing step is the same as in the first embodiment.
In the coating step, the method for coating the component (A) with the
15 component (B) is not particularly limited. The coating step has, for example, a step of
coating the component (A) with the zeolite particle group and a step of coating the
component (A) with the component (b2). Either the step of coating the component (A)
with the zeolite particle group or the step of coating the component (A) with the
component (b2} may be perfonned first. Alternatively, both of the steps may be
20 simultaneously performed. In view offurther improving the solidification inhibitor)
properties and in view of inhibiting the generation of dust, it is preferable to perform the
step of coating the component (A) with the component (b2) and then perform the step of
coating the component (A) with the zeolite particle group.
Examples of the method for coating the component (A) with the zeolite particle
25 group include the aforementioned method (11-1) in which the zeolite particle group is
5
lO
44
used instead of the component (b I).
Examples of the method for coating the component (A) with the component (b2)
include the aforementioned method (11-2) in which the zeolite particle group is used
instead of the component (b I).
As the zeolite partide group, the component (bl) may be used. In this case,
before the coating step, a selecting step of selecting, as the component (b 1 ), a zeolite
particle group having a mean particle size of equal to or greater than 0.8 J.1ffi and less than
3.8f.lm from zeolite particle groups is performed. The selecting step is the same as in
the first embodiment.
[0088]

The powder detergent of the present embodiment is the same as the powder
detergent of the first embodiment, except that the coated a-SF salt particle group of the
present embodiment (second embodiment) is used instead of the coated a-SF salt particle
15 group of the first embodiment.
20
The detergent with which the coated a-SF salt particle group of the present
embodiment is formulated is not limited to the powder detergent. For example. the
coated a-SF salt particle group may be formulated with a tabkt-typ~.: or she~:t-1) p~..· 'illliJ
detergent or a liquid detergent.
[0089]
(Third embodiment)

The group of a-sulfofatty acid alkyl ester salt particles (A) (component (A)) not
being coated with the zeolite particle group-containing coating component (B)
45
(component (B)) is easily solidified. Furthermore, the greater the content of fine
powder in the aforementioned group is, the easier it is for the solidification to occur.
However, ifthe content of the fatty acid alkyl ester in the component (A) is set to be
equal to or greater than 0.9% by mass, even ifthe group of the component (A) is
5 solidified, the component (A) is easily disintegrated (Reference Examples 3 to 5).
The a-sulfofatty acid alkyl ester salt-containing powder (hereinafter, referred to
as "a-SF salt-containing powder" as well) according to a third embodiment of the present
invention is a group of a-sulfofatty acid alkyl ester salt particles (A) (component (A)).
The content of particles (fine powder) having a particle size of equal to or less than 355
10 ~-tm in the a-SF salt-containing powder is equal to or greater than 20% by mass, and the
content of the fatty acid alkyl ester in the particles (A) is 0.9% to 4.0% by mass.
[0090]

As the component (A) in the present embodiment, the same component as the
15 component (A) in the first embodiment can be used. Her~, in th~ pr~s~nl ~mh1lJim.:nt.
the component (A) is used in which the content ofthe fatty acid alkyl ester is 0.9% to
4.0% by mass with respect to the total mass of the component (A).
In a case where the component (A) is not coated with the component (B), in
view of obtaining a-SF salt-containing powder having better solidification inhibitory
20 properties, it is preferable to increase the content of the fatty acid alkyl ester in the
component (A). The content of the fatty acid alkyl ester in the component (A) is, with
respect to the total mass of the component (A), preferably equal to or greater than I 5°JIJ
by mass, and more preferably equal to or greater than 2.0% by mass. lfthe content of
the fatty acid alkyl ester in the component (A) is the aforementioned preferred amount. it
46
is easy to obtain a-SF salt-containing powder having excellent solidification inhibitory
properties. The content of the fatty acid alkyl ester in the component (A) is, with
respect to the total mass of the component (A), preferably equal to or less than 4.0% by
mass, more preferably equal to or less than 3.5% by mass, and even more preferably
5 equal to or less than 2.5% by mass. If the content of the fatty acid alkyl ester in the
component (A) is the aforementioned preferred amount, it is easy to obtain a-Sr
salt·containing powder with a high content of an a-SF salt which is an active component.
The content of the fatty acid alkyl ester in the component (A) is, with respect to
the total mass of the component (A), preferably 1.5% to 4.0% by mass, more preferably
10 1.5% to 3.5% by mass, even more preferably 2.0% to 3.5% by mass, and panicularly
preferably 2.0% to 2.5% by mass. If the content of the fatty acid alkyl ester in the
component (A) is within the above preferred range, it is easy to obtain a-SF
salt-containing powder with excellent solidification inhibitory properties and a high
content of an active component.
15 [0091]
As the group of the component {A) in the present embodiment, it is possible to
use the same one as the group of the component (A) in the first embodiment. Here, in
the present embodiment, the group of the component (A) is used in which the content of
particles (fine powder) having a particle size of equal to or less than 355 ~min the group
20 of the component (A) is equal to or greater than 20% by mass with respect to tht total
mass of the group of the component (A).
If the content of the fine powder in the group of the component (A) is equal to or
greater than the aforementioned lower limit, in the method for manufacturing the
component (A) that will be described later, a classification operation can be skipped, and
47
the productivity is improved. In view of further improving the productivity. tlu: contcm
of the fine powder in the group of the component (A) is equal to or greater than 30% by
mass with respect to the total mass of the group of the component (A). Furthermore, the
content of the fine powder in the group ofthe component (A), with respect to the total
5 mass ofthe group of the component (A), may be 100% by mass. The content is
preferably equal to or less than 70% by mass, more preferably equal to or less than 60%
by mass, and even more preferably equal to or less than 50% by mass. If the content of
the fine powder in the group of the component (A) is equal to or less than the
aforementioned upper limit, it is easy to obtain a.-SF salt-containing powder having
10 excellent solidification inhibitory properties.
The content of the fine powder in the group of the component (A) is, with
respect to the total mass of the group of the component (A), preferably 20% to 70% by
mass, more preferably 30% to 70% by mass, even more preferably 30% to 60% by mass,
and particularly preferably 30% to 50% by mass. If the content of the fine powder in
15 the group of the component (A) is within the aforementioned preferred range, it is easy to
obtain a.~SF salt~containing powder having excellent solidification inhibitory properties.
and the productivity is improved.
20
[0092]

The method for manufacturing a.~SF salt-containing powder of the present
embodiment is the same as the method for manufacturing the component (A) in the first
embodiment.
Here, in the present embodiment, the component (A) is manufactured in which
the content of the fatty acid alkyl ester in the component (A) is 0.9% to 4.0% by mass
48
with respect to the total mass of the component (A), and the content ofthe fine powder in
the group of the component (A) is equal to or greater than 20% by mass with respect to
the total mass of the group of the component (A).
In the method for manufacturing the component (A), during the sulfonation
5 treatment, a molar ratio of a sulfonation gas to the fatty acid alkyl ester as a raw malcrial
(molar ratio represented by "sulfonation gas/fatty acid alkyl ester") is preferably 1.05 to
1.13, more preferably 1.07 to 1.11, and even more preferably 1.07 to 1.1 0. lfthe molar
ratio of sulfonation gas/fatty acid alkyl ester is within the above range, the content of the
fatty acid ester in the component (A) can be easily adjusted to be within the
10 aforementioned desired preferred range. Furthermore, it is easy to inhibit the
lengthening of the time required for the sulfonation treatment and to inhibit the decrease
in yield of the a-SF salt.
The a-SF salt-containing powder of the present embodiment has excellent
solidification inhibitory properties. Accordingly, the manufacturing method thereof
15 may not include the maturing step and/or the classifying step.
[0093}
(Fourth embodiment)
The a-SF salt-containing powder according to a fourth embodiment of the
present invention is a group of coated a-sulfofatty acid alkyl ester salt particles (coated
20 a-SF salt particles) in which the a-sulfofatty acid alkyl ester salt particles (A)
(component (A)) are coated with a zeolite particle group-containing coating ~ompdth:nt
(B) (component (B)). The content of particles (fine powder) having a particle size of
equal to or Jess than 355 f..lffi in the a-SF salt-containing powder according to the present
embodiment is equal to or greater than 20% by mass with respect to the total mass of the
49
a-SF salt-containing powder, and the content of the fatty acid alkyl ester in the
component (A) is 0.9% to 4.0% by mass with respect to the total mass of the compone-nt
(A).
The mean particle size of the coated a-SF salt-containing powder in the present
5 embodiment is the same as the mean particle size of the o:-SF salt-particle group in the
first embodiment.
10
The bulk density of the a-SF salt-containing powder in the present embodiment
is the same as the bulk density of the coated a-SF salt particle group in the first
embodiment.
[0094]

As the component (A) in the present embodiment, it is possible to use the same
one as the component (A) in the third embodiment.
[Method for manufacturing component (A)]
15 The component (A) in the present embodiment can be manufactured by the same
method as the method for manufacturing the component (A) in the first embodiment.
Here, in the present embodiment, the component (A) is manufactured in which
the content of the fatty acid alkyl ester in the component (A) is 0.9% Lo 4.0% by mass
with respect to the total mass of the component (A), and the content of fine powder in the
20 component (A) is equal to or greater than 20% by mass with respect to the total mass of
the group of the component (A).
[0095]
The content of the component (A) in the coated a-SF salt particles of the present
embodiment is the same as the content of the component (A) in the coated a.-SF salt
particles in the first embodiment.
[0096]

50
The component (B) in the present embodiment is a zeolite particle
5 group-containing coating component.
By coating the component (A) with the coating component, the solidification of
the a-SF salt-containing powder can be further inhibited.
[0097]
As the zeolite particle group of the present embodiment, it is possible to use a
10 zeolite particle group other than the component (bl) such as the commercially available
zeolite particle group shown in Table 1. In view of obtaining a better solidification
inhibitory effect, it is preferable to use the component (b 1) as the aforementioned zeolite
particle group. However, in the present embodiment, even if a zeolite partick group
other than the component (bl) is used, the solidification inhibitory effect can be obtained.
15 As the zeolite particle group other than the component (b 1 ), it is possible to preferably
use a zeolite particle group (b3) (component (b3)) having a mean particle size of3.8 to
5.0 IJ.m.
[0098]
The component (B) may contain at least one kind of component (b2) selected
20 from a fatty acid alkyl ester, a higher alcohol having 8 to 22 carbon atoms, and
polyethylene glycoL
As the component (b2), the same one as the component (b2) in the first
embodiment can be used.
The component (B) may consists of, for example, the component (b3) or the
25 component (b3) and the component (b2). Furthermore, the component (B) may contain
51
optional components other than the component (b2) and the component (b3).
[0099]
The content of the component (B) in the coated a-SF salt particles in the present
embodiment is the same as the content of the component (B) in the coated a-SF salt
5 particles of the first embodiment.
The coating ratio of the coated a-SF salt particles in the present embodiment is
the same as the coating ratio of the coated a-SF salt particles of the first embodiment.
[0100]
The content ofthe zeolite particle group in the component (B) is the same as the
10 content of the component (b 1) in the component (B) in the first embodiment.
The content ofthe zeolite particle group in the coated a-SF salt particles is the
same as the content ofthe component (bl) in coated a-SF salt particles in the first
embodiment.
[0101]
15 The content ofthe component (b2) in the component (B) is the same as the
20
content of the component (b2) in the component (B) in the first embodiment.
The content of the component (b2) in the coated a-SF salt particles is the same
as the content of the component (b2) in the coated a-SF salt particles in the first
embodiment.
[0 l 02]
In view of inhibiting the generation of dust at the time of manufacturing lhe
a-SF salt-containing powder of the present embodiment, in view of improving the
solidification inhibitory properties of the awSF salt-containing powder containing a large
amount of fine powder, and in view of improving the solidification inhibitory properties
52
in a case where the component (A) is a metastable solid, it is preferable that the
component (8) contains the component (b2).
[0 103]
In a case where the component (B) contains the component (b2), the content of
5 the zeolite particle group in the component (8), the content of the component (b2) in the
component (B), and the mass ratio of the component (b2) to the zeolite particle group in
the component (B) are the same as the content of the zeolite particle group in the
component (B), the content of the component (b2) in the component (B), and the mass
ratio of the component (b2) to the zeolite particle group in the component (B) in the
10 second embodiment respectively.
In a case where the component (B) contains the component (b2), the content of
the zeolite particle group in the coated a.-SF salt particles and the content of the
component (b2) in the coated a.-SF salt particles are the same as the content of the zeolite
particle group in the coated a.-SF salt particles and the content of the component (b2) in
15 the coated a.-SF salt particles in the second embodiment respectively.
[0104]

The method for manufacturing a.-SF salt-containing powder of the present
embodiment has a step of coating the component (A) with the component (B) (coating
20 step).
The method for manufacturing the a-SF salt-containing powder of the present
embodiment has, for example, a particle (A) manufacturing step of manufacturing the
component (A) (particles (A)) and a coating step of coating the component (A) with the
component (B).
5
lO
53
[0 105)
The particle (A) manufacturing step is a step of manufacturing the component
(A) by the same manufacturing method as the method for manufacturing the component
(A) of the first embodiment.
Here, in the present embodiment, the component (A) is manufactured in which
the content of the fatty acid alkyl ester in the component (A) is 0.9% to 4.0% hy mass
with respect to the total mass of the component (A), and the content of the fine powder in
the group of the component (A) is equal to or greater than 20% by mass with respect to
the total mass of the group of the component (A).
The a-SF salt-containing powder of the present embodiment has excellent
solidification inhibitory properties. Therefore, the manufacturing method thereof may
not include the maturing step and/or the classifying step.
[0106]
In the coating step, the method for coating the component (A) with the
15 component (B) is appropriately set according to the composition of the component (B).
Examples of the coating method used in a case where the component (B)
consists of the zeolite particle group include the method (II-1) of the first embodiment in
which the zeolite particle group is used instead ofthe component (bl).
Examples of the coating method used in a case where the component (B)
20 contains the component (b2) include the same method as the coating step of the second
embodiment.
In the present embodiment, the component (b 1) may be used as the zeolite
particle group. In this case, before the coating step, a se1ecting step of selecting. as the
component (b 1 ), a zeolite particle group having a mean particle size of equal to or greater
25 than 0.8 j..Ull and less than 3.8 ~m from zeolite particle groups is performed. The
54
selecting step is the same as in the first embodiment.
[0107]

The powder detergent containing the a.-SF salt-containing powder of the third
5 embodiment or the a-SF salt-containing powder of the fourth embodiment is the same as
the powder detergent of the first embodiment, except that, instead of the coated a-SF salt
particle group of the first embodiment, the a-SF salt-containing particles ofthe third
embodiment or the a-SF salt-containing powder of the fourth embodiment is used.
The detergent with which the a-SF salt-containing powder of the third
10 embodiment or the a-SF salt-containing powder of the fourth embodiment is formulated
is not limited to the powder detergent. For example, the a-SF salt-containing powder
may be formulated with a tablet-type or sheet-type solid detergent or a 1iquid detergent.
[0108]
As described so far, the coated a-SF salt particle group of the present invention
15 consists of the coated a-SF salt partic1es coated with a specific component (B).
Accordingly, the solidification inhibitory properties of the coated a-SF salt particle group
are excellent.
The coated a-SF salt particle group or the a-SF salt-containing powder of the
present invention contains the component (A) in which the content of the fatty acid alkyl
20 ester is 0.9% to 4.0% by mass. Accordingly, the solidi lication inhibitory propt!rtit!s of
the coated a.-SF salt particle group or the a.-SF salt-containing powder are excellent.
[Examples]
[0109]
Hereinafter, the present invention will be more specifically described using
5
55
examples, but the present invention is not limited to the examples. In the present
examples, unless otherwise specified, "%" represents "% by mass".
The raw materials used in the present examples are as below.
[0 110]

Tables 2 to 4 show the composition of a-1 to a-22 as groups of the component
(A) used in the present examples, the amount of fine powder in a-1 to a-22, a degree of
crystallinity, and a reaction molar ratio of S03/fatty acid methyl ester at the time of
preparing a-1 to a-22.
10 For reference, particle size distributions ofa-1 (amountoffine powder: 15% by
15
mass) and a-10 (amount of fine powder; 40% by mass) are shown in Table 5.
a-1 to a-22 are groups of a-SF salt particles represented by Formula (l)
described above in which R1 is an alkyl group having 14 to 16 carbon atoms, R2 is a
methyl group, and M is sodium.
The method for preparing a-1 to a-22, the method for analyzing th~ composition
thereof, and the method for measuring the degree of crystallinity are as described below.
[0 Ill J
(Table 2]
AI
(Di-Na salt)
Sodium sulfate
Sodium methyl
Composition
sulfate
(%by mass) Fatty acid
methyl ester
(ME)
Moisture
Others
Total
Amount of fine powder (% by
mass)
Degree of crysta11inity (%)
Reaction molar ratio of
SO)~" fatty acid methyl ester
56
a-1 a-2
91.3 91.3
(4.6) (4.6)
1.2 1.2
3.8 3.8
0.6 0.6
2.2 2.2
0.9 0.9
100 100
15 20
75 75
1.15 l.15
a-3 a-4 a-5 a-6
91.3 91.3 91.3 91.3
(4.6) (4.6) (4.6) (4.6)
l.2 1.2 1.2 1.2
3.8 3.8 3.8 3.8
0.6 0.6 0.6 0.6
2.2 2.2 2.2 2.2
0.9 0.9 0.9 0.9
100 100 100 100
30 40 50 15
75 75 75 20
1.15 1.15 1.15 1.15
[0112]
[Table 3]
AI
(Di-Na salt)
Sodium
sulfate
Sodium
Composition
methyl
sulfate
(%by mass) Fatty acid
methyl ester
(ME)
Moisture
Others
Total
Amount of fine powder (%
by mass)
Degree of crystallinity (%)
Reaction molar ratio of
SOifatty acid methyl ester
57
a-7 a-8 a-9
91.6 90.7 86.4
(6.3) (6.6) (5.8)
1.0 1.1 1.3
2.8 2.4 3.7
1.3 1.9 3.4
2.1 2.1 2.7
1.2 1.8 2.5
100 100 100
40 40 40
75 73 76
1.11 1.07 1.05
a-10 a-ll a-12 a-13 a-14 a-1 5
90.2 91.2 91.3 90.7 90.8 86.4
(5.8) (5.7) (4.6) (5.8) (6.0) (5.8)
1.2 1.2 1.2 1.1 1.1 1.3
3.2 2.8 3.8 2.9 2.9 3.7
1.1 1.3 0.6 1.2 1.4 3.4
2.6 2.1 2.2 2.3 2.3 2.7
1.7 1.4 0.9 1.8 1.5 2.5
100 100 100 100 100 100
40 40 40 40 40 40
50 57 20 40 22 23
1.13 l.ll 1.15 1.12 1.10 1.05
[0113]
[Table 4]
AI
(Di-Na salt)
Sodium sulfate
Sodium methyl
Composition
sulfate
(%by mass) Fatty acid
methyl ester
(ME)
Moisture
Others
Total
Amount of fine powder (% by
mass)
Degree of crystallinity(%)
Reaction molar ratio of
S03/fatty acid methyl ester
58
a-16 a-17
91.3 90.7
(4.6) (6.6)
1.2 l.l
3.8 2.4
0.6 I .9
2.2 2.1
0.9 1.8
100 100
100 100
81 76
1.15 1.07
a-18 a-19 a-20 a-21 a-22
86.4 90.7 86.4 90.7 86.4
(5.8) _{_6.6)_ (5.8) (6.61 (5.8)
1.3 1.1 1.3 1.1 1.3
3.7 2.4 3.7 2.4 3.7
3.4 1.9 3.4 1.9 3.4
2.7 2.1 2.7 2.1 2.7
2.5 1.8 2.5 1.8 2.5
100 100 100 100 100
100 20 20 30 30
76 73 76 73 76
1.05 1.07 1.05 1.07 1.05
59
[0114]
[Table 5]
a-1 a-10
1400 j.lffi. on 0.1 0.2
1180 11m. on 2.2 2.4
1000 J.lffi. on 4.4 5.3
710 1-1m. on 30.0 17.9
Particle size
distribution 500 1-1m. on 30.2 19.8
(%by mass)
355 ).Ull. on 18.1 14.3
250 J.I.ID. on 3.8 13.8
150 11m. on 4.8 14.0
150 J..lffi. pass 6.4 12.4
355 ~J.m, pass (amount of fine 15.0 40.2
powder'
Particle size 250 ~-~.m. on 25.3 34.3
distribution of fine
powder 150 1-1m. on 32.0 34.8
(%by mass) 150 1-1m. pass 42.7 30.9
[0115]
a-1 to a-22 are as prepared as below.
5 (Method for preparing a-1 to a-5)
[Paste preparing step]
Methyl palmitate (manufactured by Lion Corporation, trade name "PASTEL
M-16") and methyl stearate (manufactured by Lion Corporation, trade name "PASTEL
M-180") were mixed together at 80:20 (mass ratio).
10 330 kg of the aforementioned fatty acid methyl ester mixture and anhydrous
sodium sulfate as a coloration inhibitor, which was in an amount of 5% by mass with
respect to the fatty acid methyl ester mixture, were put into a reaction device having a
60
volume of 1 kL equipped with a stirrer. While the resultant was being stirred, 110 kg of
so3 gas (sulfonation gas) diluted with 4% by volume of nitrogen gas was blown
thereinto over 3 hours at a constant velocity with bubbling so as to cause a reaction.
The reaction temperature was kept at 80°C. The molar ratio of the sulfonation gas to
5 the fatty acid methyl ester mixture (sulfonation gas/fatty acid methyl ester mixture) was
1.15.
The above reactant was moved to an esterification tank, and 14 kg of methanol
was supplied thereto, thereby causing an esterification reaction at 80°C. The esterified
substance obtained after the reaction was extracted from the esterification tank, and an
10 equivalent amount of an aqueous sodium hydroxide solution was added thereto by using
a line mixer, thereby continuously neutralizing the esterified substance.
Then, the neutralized substance was injected into a bleaching agent mixing line,
35% aqueous hydrogen peroxide was supplied thereto in an amount of 1% to 2% by mass
with respect to the a.-SF salt in tenns of a pure content, and the aqueous hydrogen
15 peroxide was mixed with the a-SF salt in a state where the temperature was being kept at
80°C, thereby obtaining an a-SF salt-containing paste.
[0 116]
[Flaking step 1
The obtained a-SF salt-containing paste was introduced into a vacuum thin-film
20 evaporator (heat-transfer surface: 4m2
, manufactured by Ballestra) at 200 kg/hr,
concentrated at an inner wall heating temperature of 1 oooc to 160°C and a degree of
vacuum of 0.01 to 0.03 MPa, and extracted as a melt with a temperature of I oooc to
130°C.
The melt was cooled to 20°C to 30°C for 0.5 minutes by using a belt cooler
5
10
15
20
61
(manufactured by NIPPON BELTING CO., LTD.). Subsequently, by using a
disintegrator (manufactured by NIPPON BELTING CO., LTD.), a-SF salt-containing
flakes were obtained.
[0117]
[Maturing step]
A 1 m3 flexible container bag was filled with 600 kg of the a-SF salt-containing
flakes and held in an environment with a temperature of 30°C for 4 weeks, thereby
converting the a-SF salt-containing flakes into stable solids.
[0118]
[Grinding step]
The flakes were put into a grinder (Fitzmill) and ground at 1,300 rpm, thereby
obtaining a-SF salt particles.
[0119]
[Classifying step]
The obtained group of the a-SF salt particles was sieved using a sieve with 355
Jlm apertures, and fine powder passing through the sieve was cut. Then, the cut fine
powder was returned to (mixed with) the a-SF salt particles such that the particles
contained a predetermined amount of fine powder, thereby preparing a-1 to a-5.
[0120]
(Method for preparing a-6 and a-12)
a-6 and a-12 were prepared in the same manner as used for rreparing a-1 to a-5.
except that, after the a-SF salt-containing flakes were obtained, the maturing step was
not performed.
[0121]
5
62
(Method for preparing a-7)
a-7 was prepared in the same manner as used for preparing a-1 to a-5. except
that, in the paste preparation step, the molar ratio of the sultonation gas to the huty acid
me thy I ester mixture ( sulfonation gas/fatty acid me thy I ester mixture) was set to be 1.11.
[0122]
(Method for preparing a-8, a-19, and a-21)
a-8, a-19, and a-21 were prepared in the same manner as used for preparing a-1
to a-5. except that, in the paste preparation step, the molar ratio of the sulfonation gas to
the fatty acid methyl ester mixture (sulfonation gas/fatty acid methyl ester mixture) was
10 setto be 1.07.
[0123]
(Method for preparing a-9, a-20, and a-22)
a-9, a-20, and a-22 were prepared in the same manner as used for preparing a-1
to a-5, except that, in the paste preparation step, the molar ratio of the sulfonation gas to
15 the fatty acid methyl ester mixture (sulfonation gas/fatty acid methyl ester mixture) was
set to be 1.05.
[0124]
(Method for preparing a-1 0)
a-10 was prepared in the same manner as used for preparing a-1 to a-:'i. ex~.:l.?pt
20 that, in the paste preparing step, the molar ratio of the sulfonation gas to the fatty acid
methyl ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be 1.13,
and in the maturing step, the a-SF salt-containing flakes were kept for 2 weeks in an
environment with a temperature of equal to or higher than 30°C.
[01251
25 (Method for preparing a-ll)
5
63
a-ll was prepared in the same manner as used for preparing a-7, except that, in
the maturing step, the a-SF saJt-containing flakes were kept for 2 weeks in an
environment with a temperature of equaJ to or higher than 30°C.
[0126]
(Method for preparing a-13)
a-13 was prepared in the same manner as used for preparing a-1 to a-5. C'lcert
that, in the paste preparing step, the molar ratio of the sulfonation gas to the fatty acid
methyl ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be I. 12,
and in the maturing step, the a-SF salt-containing flakes were kept for I weeks in an
lO environment with a temperature of equaJ to or higher than 30°C.
[0127]
(Method for preparing a-14)
a-14 was prepared in the same manner as used for a-6 and a-12. except that. in
the paste preparing step, the molar ratio of the sulfonation gas to the fatty acid methyl
15 ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be 1.10.
[0128]
(Method for preparing a-15)
a-15 was prepared in the same manner as used for preparing a-14, except that, in
the paste preparing step, the molar ratio of the sulfonation gas to the fatty acid methyl
20 ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be 1.05.
[0129]
(Method for preparing a-16)
In the same manner as used for preparing a-1 to a-5. the flaking step. th~.!
maturing step, and the grinding step were performed. Then, in the classitYing st~p. th~
64
group of the a.-SF salt particles was sieved using a sieve with apertures with a size of 355
)lm, and the fine powder passing through the sieve was collected, thereby preparing a-16.
[0130]
(Method for preparing a-17)
5 a-17 was prepared in the same manner as used for preparing a-16, except that, in
10
the paste preparing step, the molar ratio of the sulfonation gas to the fatty acid methyl
ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be 1.07.
[0131]
(Method for preparing a-18)
a-18 was prepared in the same manner as used for preparing a-16, except that, in
the paste preparing step, the molar ratio ofthe sulfonation gas to the fatty ac1d lllt.:tllyl
ester mixture (sulfonation gas/fatty acid methyl ester mixture) was set to be 1.05.
[0132]
(Method for measuring degree of crystallinity)
I 5 As a differential scanning calorimeter, DSC6220 manufactured by Seiko
20
Instruments lnc was used. 20 g of a sample was ground using a TRIO BLENDER
(manufactured by Trio Science Co., Ltd.), and 5 to 30 mg of the obtained resultant was
put into a sample pan made of silver, heated to 130°C from ooc at a rate of2°C/min, and
thermally analyzed.
At this time, from a heat absorption peak areaS l at a temperature of 50°C
130°C and a heat absorption peak area S2 at a temperature of0°C to l30°C, the value of
100 x Sl/S2 was determined and taken as a degree of crystallinity(%). Each of the area
Sl and the area S2 was detennined by performing "automatic splitting time integration"
by using the software attached to the differential scanning calorimeter. If an exothermic
65
peak was checked at a temperature of 50°C to 130°C, a value obtained by subtracting the
absolute value of the exothermic peak from the heat absorption peak area at a
temperature of 50°C to 130°C was taken as S 1. 1 fan exothermic peak was checked at a
temperature of0°C to l30°C, a value obtained by subtracting the absolute value of the
5 exothermic peak from the heat absorption peak area at a temperature of 0°C to 13 0°C
was taken as S2.
10
(0133]
(Method for analyzing compositions of a-1 to a-22)
The compositions of a-1 to a-22 were analyzed as below.
[0134]
[Method for measuring AI]
The total content (AI) ofthe a -SF salt and the a-sul fofatty acid dialkali salt
(Di-Na salt) was measured as below.
The a-SF salt-containing flakes (for a-1 to a-5, a-7 to a-11, a-13, and a-16 to
15 a-22, the flakes obtained after the maturing step; for a-6, a-12, a-14, and a-15, the flakes
obtained after the flaking step; the same shall be applied to the following measurement
method) was accurately weighed out in an amount of about 0.2 g into a volumetric flask
having a volume of200 mL, deionized water (di stilled water) was add~.:d tiKrl'ln up ll) a
gauge line, and the sample was dissolved in the deionized water by using ultrasonic
20 waves. After being dissolved, the sample was cooled to a temperature of about 25°C, 5
mL ofthe aqueous solution of the sample was moved to a titration bottle by using a hole
pipette, and 25 mL of a methylene blue indicator and 15 mL of chloroform were added
thereto. Thereafter, 5 mL of 0.004 mol/L benzethonium chloride solution was added
thereto, and then titration was performed using a 0.002 moi/L sodium alkylbenzene
5
66
sulfonate solution. Whenever the titration was perfonned, the titration bottle was caped,
vigorously shaken, and then allowed to stand. At a point in time when the colors of two
separating layers were found to be the same as each other against a white board in the
background was regarded as being the end point of the titration.
In the same manner as described above, a blank test (performed in the same
manner as described above except that the sample was not used) was performed, and
from a difference of a titration amount ofthe sodium aJkylbenzene sulfonate solution, the
content of Al in the component (A) was calculated from the following equation.
AI content(% by mass)"" (titration amount in blank test (mL)- titration amount
10 (mL)) x 0.002 (mol/L) x content of a-SF salt/( amount of sample collected (g) x 5
(mL)/200 (mL))/1 0
[0135]
[Method for measuring content of a-sulfofatty acid dia1kali salt (Di-Na salt)]
The content of the a-sulfofatty acid dialkali salt in the component (A) was
15 measured as below.
A standard a-s.ulfofatty acid dialkali salt was accurately weighed out in an
amount of0.02 g, 0.05 g, and 0.1 g respectively into a volumetric ilask having a volume
of 200 mL, water in an amount of about 50 mL and ethanol in an amount of about 50 mL
were added thereto, and the salt was dissolved using ultrasonic waves. After being
20 dissolved, the salt was cooled to a temperature of about 25°C, methanol was added
thereto accurately up to a gauge line, and the resultant was taken as a standard solution.
The standard solution in an amount of about 2 mL was filtered using a 0.45 ~Lm
chromatographic disk and analyzed by high-performance liquid chromatography under
the following measurement conditions. From the peak area, a calibration curve was
5
10
plotted.
67
<>
-Device: LC-6A (manufactured by Shimadzu Corporation)
·Column: Nucleosil SSB (manufactured by GL Sciences Inc.)
·Column temperature: 40°C
-Detector: differential refractive index detector RID-6A (manufactured by
Shimadzu Corporation)
solution
·Mobile phase: H20 of 0.7% sodium perchlorate/CH30H = 114 (volume ratio)
·Flow rate: 1.0 mL/min
·Injection amount 100 IlL
Thereafter, the a.-SF salt-containing flakes were accurately weighed out in an
amount of about 0.8 g into a volumetric flask having a volume of200 mL water in an
amount of about 50 mL and ethanol in an amount of about 50 mL were added thl.!rcto,
15 and the flakes were dissolved. After dissolution, the solutoin was cooled to a
temperature of about 25°C, methanol was added thereto accurately up to a gauge line,
and the resultant was taken as a sample solution. The sample solution in an amount of
about 2 mL was filtered using a 0.45 1-1m chromatographic disk and analyzed by
high-performance liquid chromatography under the same conditions as dcscrib~o:d above.
20 By using the aforementioned calibration curve, the concentration u r th~ u.-sulli.\ratt~ ac1d
dialkali salt in the sample solution was determiend, and the cotncnt (%by mass) of the
a-sulfofatty acid dialkali salt in the component (A) was calcuated.
[0136]
[Method for measuring content of sodium sulfate and sodium methyl sulfate]
68
The contentofsodium sulfate and sodium methyl sulfate in the compont:nt (/\)
was measured as below.
Each of the standard sodium sulfate and the standard sodium methyl sulfate was
accurately weighed out in an amount ofO.Ol g, 0.02 g, 0.05 g, and 0.1 g into a volumetric
5 flask having a volume of 1,000 mL, deionized water (distilled water) was added thereto
up to a gauge line, and dissolution was performed using ultrasonic waves. After the
dissolution, the solutoin was cooled to a temperature of about 25°C, and the resultant was
taken as a standard solution. The standard solution in an amount of about 2 mL was
filtered using a 0.45 J..l.ffi chromotographic disk and subjected to ion chromatography
10 under the following measurement conditions~ and from peak areas of the standard
solutions ofthe sodium methyl sulfate and the sodium sulfate, calibration curves were
plotted.
15
20
<>
·Device: DX-500 (manufactured by Nippon Dionex K. K.)
·Detector: conductivity detector CD-20 (manufactured by Nippon Dionex K. K.)
·Pump: IP-25 (manufactured by Nippon Dionex K. K.)
·Oven: LC-25 (manufactured by Nippon Dionex K. K.))
·Integrator: C-R6A (manufactured by Shimadzu Corporation)
·Separation column: AS-12A (manufactured by Nippon Dionex K. K.))
·Guard column: AG-12A (manufactured by Nippon Dionex K. K.)
·Eluent: aqueous solution of2.5 mM Na2C03/2.5 mM NaOH/5% (volume)
acetonitrile
·Flow rate of eluent: 1.3 mL/min
·Regenerating liquid: pure water
·Column temperature: 30°C
-Loop volume: 25 ~L
[0137]
69
Then, a-SF salt-containing flakes were accurately weighed out in an amount of
5 about 0.2 g into a 200 mL volumetric flaks, deionized water (distilled water) was added
thereto up to a gauge line, and dissolution was perform~:<.! using ultrasunic \\ iJ\ cs. :\ lkr
the dissolution, the solution was cooled to a temperature of about 25°C and taken as a
sample solution. The sample solution in an amount of about 2 mL was filtered using a
0.45 ~m chromatographic disk and analyzed by ion chromatography under the same
10 measurement conditions as described above. By using the calibration curve plotted as
above, the concentration of the sodium sulfate and the concentration of the sodium
methyl sulfate in the sample solution were determined, and the content(% by mass) of
the sodium sulfate and the content of the sodium methyl sulfate in the component (J\)
were calculated.
15 [0138]
[Method for measuring content of fatty acid methyl ester (ME)J
The content of the fatty acid methyl ester in the component (A) was measured as
below. A standard fatty acid methyl ester was accurately weighed out in an amount of
0. 02 g, 0.10 g, and 0.20 g respectively into a volumetric flask having a volume of 50 mL,
20 methanol was added thereto up to a gauge line, and dissolution was performed using
ultrasonic waves. After the dissolution, the solution was cooled to a temperature of
about 25°C and taken as a standard sol uti on. Tht: standard solution in an amount u r
about 2 mL was filtered using a 0.45 ~m chromatographic disk and subjected to
high-performance liquid chromatography under the following measurement conditions.
5
10
70
From the peak area thereof, a calibration curve was plotted.
<>
·Device: LC-1 OAT (manufactured by Shimadzu Corporation)
-Column: Inertsil ODS-2 (manufactured by GL Sciences Inc.)
·Column temperature: 40°C
-Detector: differential refractive index detector RID-6A (manufactured by
Shimadzu Corporation)
·Mobile phase: mixed solution ofH20/CH30H = 5/95 (volume ratio)
-Flow rate: 1.0 mL/min
·Injection amount 100 ).lL
Thereafter, a-SF salt-containing flakes were accurately weighed out in an
amount of about 4.0 g into a volumetric flask having a volume of 50 mL, methanol was
added thereto up to a gauge line, and dissolution was performed using ultrasonic waves.
After the dissolution, the resultant was cooled to a temperature of about 25°C and taken
15 as a sample solution. The sample solution in an amount of about 2 mL was filtered
using a 0.45 ).lm chromatographic disk and then subjected to high-performance liquid
chromatography under the same measurement conditions as described above. By using
the aforementioned calibration curve, the concentration of the fatty acid methyl ester in
the sample solution was detennined, and the content(% by mass) of the fatty acid methyl
20 ester in the component (A) was calculated.
[0139]
[Method for measuring moisture amount: Karl Fischer method]
The cx.-SF salt-containing flakes were made into a ground substance by being
finely ground. The ground substance was collected in an amount of about 0.05 g, the
5
10
15
71
moisture amount in the ground substance was measured using a Karl Fischer moisture
meter MKC-210 (manufactured by KYOTO ELECTRONICS MANUFACTUlUNU CO.,
LTD.), and the moisture amount(% by mass) in the component (A) was calculated.
[0 140]

bl-1: A-type zeolite (mean particle size: 1.0 ~m)
bl-2: A-type zeolite (mean particle size: 2.5 ~Jill)
bl-3: A-type zeolite (mean particle size: 2.7 ~m)
bl-4: A-type zeolite (mean particle size: 3.4 J.Lm)

b 1 '-1: A-type zeolite (mean particle size: 0.5 J.LID)
bl '-2: A-type zeolite (mean particle size: 4.0 J.Lm), manufactured by Guangzhou
Hengbang Fine Chemical Co., Ltd., 4A zeolite
bl-1 to bl-4 and bl '-1 were prepared by grinding 4A /.~ulit~ (mean panich.: sit . .:
4.0 J.Lffi) manufactured by Guangzhou Hengbang Fine Chemical Co., Ltd used as b 1·-2 by
using a mortar such that the zeolite had a predetermined mean particle size.

b2-1: ME, fatty acid methyl ester (number of carbon atoms of the fatty acid: 16
20 to 18), manufactured by Emery oleochemicals, Cl6/C18 = 85115 (mass ratio)
[0141]

[Examples 1 to 12 and 25 to 33, Comparative Exampks 1 to 7, and Re1Cn:n<:~
72
Examples 6 to 11]
According to the compositions shown in Tables 6, 8, and 10, the group of the
component (A) and the component (bl) were put into a container rotation-type mixer
such that the components were mixed together, thereby obtaining coated a.-SF salt
5 particle groups of Examples I to 12 and 25 to 33.
Coated a-SF salt particle groups of Comparative Examples I to 7 and Reference
examples 6 to 11 were obtained in the same manner as described above, except that the
(bl ')component was used instead of the component (bl). The coated a.-SF salt particle
groups of Reference examples 6 to II are examples of the a-SF salt-containing powder
10 ofthe fourth embodiment described above, and the component (bl '-2) used in these
examples corresponds to the (b3) component of the fourth embodiment.
[Examples 13 to 24 and Reference Examples I and 2]
According to the composition shown in Table 7, the group of the component (A)
was put into the container rotation-type mixer, and in a state where the group of the
15 component (A) was flowing, the component (b2) was sprayed thereto. After the
spraying of the component (b2) was finished, the component (b 1) or the (b 1 ') component
was put into the mixer such that the components were mixed together, thereby obtaining
coated a-SF salt particle groups of Examples 13 to 24 and Reference Examples 1 and 2.
20
[Reference Examples 3 to 5]
As Reference Examples 3 to 5, a-16 to a-18 were used as they are (the Rdcrem.:t:
Examples 4 and 5 are examples of the coated a-SF salt particles ofthe third embodiment
described above. Hereinafter, the coated a-SF salt particle groups of Refen.:n\:1..'
Examples 3 to 5 will be referred to as coated a-SF salt particle groups as in other
examples).
5
73
Tables 6 to 10 show the composition of the obtained coated a-SF salt particle
groups (fonnulation component and content (part by mass)).
If the column of the formulation component in the table remains blank. it means
that the formulation component is not formulated.
[0142]
For the coated a-SF salt particle group of each example, the content of fine
powder (particles having a particle size of equal to or less than 355 ~m) was measured as
below. The measurement results are shown in Tables 6 to I 0.
Furthermore, for the coated a-SF salt particle group of each example. the
10 solidification inhibitory properties were evaluated as below. The evaluation results are
shown in Tables 6 to 10.
[0143]
[Measurement of content of fine powder]
The coated a-SF salt particle group of each example was sieved using a sieve
15 having apertures with a size of355 ~m. and from the amount of fine powder passing
through the sieve, the content of the fine powder was calculated by the following
equation.
20
Content of fine powder(% by mass)= (mass of fine powder passing through
sieve/total mass of coated a-SF salt particle group remaining on the sieve) x 100
[0144]
[Evaluation of solidification inhibitory properties]
The solidification inhibitory properties of the coated a-SF salt particle group of
each example were evaJuated by the following solidification index.
<>
5
74
85 parts by mass of a-l and 15 parts by mass of b l '-2 were put into the
container rotation-type mixer such that they were mixed together, thereby obtaining a
coated a-SF salt particle group. The coated a-SF sa1t particle group was taken as a
standard sample.
80 g of the standard sample was put into a cylindrical cell having an inner
diameter of 50 mm and a height of 100 mm and allowed to stand for 1 week under a load
of2 kg in an environment with a temperature of 40°C, thereby obtaining a cylindrical
molded materia1. The molded material was taken out, and by using a FORCE GAUGE
(model No. body: t-AX-SOON, detection portion: ZP-500N) manufactured by IMDA~
10 Incorporated, the detection portion was lowered from the upper portion under a condition
15
of5.32 m.mfsec. A load was slowly imposed on the entirety ofthe upper surface ofthe
molded materia1, and a maximum load (kgf) applied thereto until the molded material
was destroyed was measured. The maximum load was measured 3 times, and the
average (Wo) thereof was determined.
In the same manner as described above, a cylindrical molded material of the
coated a-SF sa1t particle group of each example was obtained. Then, in the same
manner as described above, a maximum load (kgf) applied thereto until the molded
material was destroyed was measured. For each molded material, the maximum load
was measured 3 times, and the average (W1) of the maximum loads measured 3 times
20 was determined for each example.
Then, by the following equation, a solidification index wa'> calculated.
Solidification index= 10 x (W 1/Wo)
The smaller the solidification index is, the better the evaluation result of
solidification inhibitory properties can be.
75
[0145]
[Table 6]
Examples
1 2 3 4 5 6 7 8 9 10 11 12
a-1 85 85 85
a-2 85 85
Group of component (A) a-3 85 85
a-4 85
a-5 85 85 85 .
Composition a-6 85 '
(part by b 1-1 15
mass) Component b1-2 15 15 15 15
Component (b 1) bl-3 15 15 15 15 15 15
(B) bl-4 15
Component bl '-1
(bl ') bl '-2
Total 100 100 100 100 100 100 100 100 100 100 100 100
Content of fme powder (% by mass) 17 17 22 32 53 17 23 31 40 52 50 17
Solidification index 1 2 3 5 11 6 8_ j_O 11 14 13 10 !
- -
[0146]
[Table 7]
Group of component
(A)
~omposition
(part by ~omponen
mass) (b1)
Component
(B) Componen
(b2)
~omponent
(bl ')
Total
a-1
a-2
a-3
a-4
a-5
a-6
bl-1
bl-2
bl-3
bl-4
b2-1
b 1 '-1
bl '-2
Content of fine powder (% by mass)
Solidification index
13
85
15
0.5
100.5
15
6
76
Examples
14 15 16 17
85
85
85
85
15 15 IS 15
0.5 0.5 0.5 0.5
100.5 100.5 100.5 100.5
20 30 40 51
7 9 10 12 -·
Reference
Examples
Examples
18 19 20 21 22 1 2 23 24
85
85
85 85 85
85
85
85 85
15 15 15 15 15 15 15
1.0 1.0 l.O 1.0 1.0 0.5 1.0 0.5 1.0
15 15
101 101 101 101 101 100.5 101 100.5 101
13 19 31 42 50 33 31 14 14 i
4 7 9 ll 12 14 13 4 1 !
[0147]
[Table 8]
Group of component (A)
Composition
(part by mass)
Component
Component (bl)
(B)
Component
(bl ')
Total
Content of tine powder(% by mass}
Solidification index
77
I 2
a-1 85 85
a-2
a-3
a-4
a-5
a-6
b1-1
bl-2
bl-3
bl-4
bl , ·l 15
bl '·2 15
100 100
17 16
28 10 - ..
Comparative Examples
3 4 5 6 7
85
85
85
85
85
15 15 15 15 15
100 100 100 100 100
20 30 40 51 17
12 15 21 25 21
78
[0148]
[Table 9]
Examples
25 26 27 28 29 30 31 32 33
a-7 85
a-8 85
a-9 85
a-10 85
Group of component (A) a-ll 85
a-12 85
a-13 85
Composition a-14 85
(part by mass) a-15 85
b 1-1
Component bl-2
Component (b 1) bl-3 15 IS 15 15 15 15 15 I 5 15
(B) bl-4
Component bl, -1
(b I ') bl '-2
Total 100 100 100 100 100 100 100 100 100
Content of fine powder(% by mass) 40 40 40 40 40 40 40 40 40
Solidification index 9 8 7 12 11 19 12 !0 4 - --- --
[0149]
[Table 10]
Group of component (A)
Composition
(part by mass)
Component
Component (bl)
(B)
Component
(bl ')
Total
Content of fine powder(% by mass)
Solidification index
a-16
a-17
a-18
a-19
a-20
a-21
a-22
a-8
a-9
b 1-1
bl-2
bl-3
bl-4
b1 '-1
bl'-2
79
3 4 5
85
85
85
85 85 85
100 100 100
82 62 44
Reference Examples
6 7 8 9 10 11
85
85
85
85
85
85
15 15 15 15 15 IS
100 100 100 100 100 100
20 20 30 30 40 40
11 7 15 9 17 10_ --.
80
[0150}
From the results shown in Tables 6 to 10, it can be confirmed that the coated
a.-SF salt particle groups of Examples l to 33 to which the present invention is applied
have excellent solidification inhibitory properties.
5 Through the comparison between Examples 1 to 12 and Comparative Examples
1 to 7, it can be confirmed that the use of the component (b 1 ), having a mean particle size
within a specific range, as the component (B) can improve the solidification inhibitory
properties.
From the Examples 13 to 24 and Reference Examples 1 and 2, it can be
l 0 confirmed that, if the component (B) contains the component (b2), the solidification
inhibitory properties can be improved. Although Examples 23 and 24 are coated a.-SF
salt particle groups using the component (A) having a degree of crystallinity of less than
50%, the solidification inhibitory properties there are excellent.
From Examples 25 to 33 and Reference Examples 3 to 11, it can be confirmed
15 that the coated a-SF salt particle group in which the content of the fatty acid methyl ester
in the component (A) is 0.9% to 4.0% by mass has excellent solidification inhibitory
properties. Furthermore, it can be confirmed that, if the content of the fatty acid methyl
ester is high within the aforementioned range of the content, the solidification inhibitory
properties are excellent. In addition, it can be confirmed that, in the coated a-SF salt
20 particle group using the component (A) having a degree of crystallinity of less than 50%,
the effect of improving the solidification inhibitory properties can be more rei iably
exhibited.
In contrast, in the coated a.-SF salt particle group (Comparative Example l)
using the component (bl '-1) instead ofthe component (bl), the component (bl '-1) itself
81
was aggregated, the effect of the particle size could not be obtained, and the solidification
inhibitory properties were not obtained. As is evident from the comparison between
Comparative Examples 2 to 6 and, for example, Example 2, Comparative Example 2,
Example 3, Comparative Example 3, and the like coated with the same component (A),
5 all of the coated a.-SF salt particle groups (Comparative Examples 2 to 6) using the
component (b 1 '-2) instead of the component (bl) were poorer in tenns of the
solidification inhibitory properties than the coated a.-SF salt particle group to which the
present invention was applied.
From the above results, it could be confirmed that the coated a.-SF salt particle
10 group to which the present invention is applied has excellent solidification inhibitory
properties.
[Industrial applicability]
[0 151]
The coated a.-SF salt particle group to which the present invention is applied can
15 be used in a powder detergent and the like.

CLAIMS
1. A coated a.-su1fofatty acid alkyl ester salt particle group comprising:
a.-sulfofatty acid alkyl ester salt particles (A)~ and
a zeolite particle group-containing coating component (B) with which the
particles (A) are coated,
wherein the zeolite particle group is a zeolite particle group (bl) having a mean
particle size of equal to or greater than 0.8 j..lffi and less than 3.81Jm.
2. The coated a-sulfofatty acid alkyl ester salt particle group according to
claim 1,
wherein a content of the fatty acid alkyl ester in the particles (A} is 0.9% to
4.0% by mass, and
a content of particles having a particle size of equal to or less than 355 J.1In in the
15 coated a-sulfofatty acid alkyl ester salt particle group is equal to or greater than 20% by
mass.
20
3. The coated a.-sulfofatty acid alkyl ester salt particle group according to
claim I or 2,
wherein when the particles (A) are thermally analyzed using a differential
scanning calorimeter, an observed heat absorption peak area Sl at a temperature of 50°C
to 130°C is less than 50% of a heat absorption peak area S2 at a temperature of0°C to
130°C.
5
83
4. A powder detergent comprising:
the coated a-sulfofatty acid alkyl ester salt particle group according to any one
of claims 1 to 3.
5. A method for manufacturing the coated a-sulfofatty acid alkyl ester salt
particle group according to any one of claims 1 to 3, comprising:
a step of coating the a-sulfofatty acid alkyl ester salt particles (A) with the
zeolite particle group-containing coating component (B).
wherein the zeolite particle group is a zeolite particle group (b 1) having a mean
10 particle size of equal to or greater than 0.8 ~m and less than 3.8 ~m.
6. The method for manufacturing the coated a-sulfofatty acid alkyl ester salt
particle group according to claim 5,
wherein a content of particles having a particle size of equal to or less than 355
15 ~m in the particle group constituted with the particles (A) is equal to or greater than 20%
by mass, and
20
a content of the fatty acid alkyl ester in the particles (A) is 0.9% to 4.0% by
mass.
7. The method for manufacturing the coated a-sulfofatty acid alkyl ester salt
particle group according to claim 5 or 6, further comprising:
a particle {A) manufacturing step of manufacturing the particles (A),
wherein the particle (A) manufacturing step includes a sulfonation treatment for
causing sulfonation by bringing the fatty acid alkyl ester into contact with a sulfonation gas,and a molar ratio of the sulfonation gas to the fatty acid alkyl ester in the sulfonation treatment is 1.05 to 1.13.