The present invention relate to an emulsion formulation for colour deepening of different types textile fabrics and fibers and in particular to an emulsion formulation for colour deepening of textile fabrics/fibres without any undesirable colour shade development on the textiles and fibers specially in case of synthetic fiber or fabric after colour deepening treatment. Importantly, the emulsion is also suitable to resist thermal migration especially for synthetic fabric and adapted to also impart excellent soft hand and surface feeling on the treated fabrics and fibers.
Background Art
Synthetic fabric or fiber, especially polyester fabric or fiber has always a problem of awful colour depthness after treating the fabric or fiber with disperse dye. In fabric processing house, it is a chronic problem faced by textile chemists during their regular activities of polyester fabric or fiber dyeing steps. This usually requires redyeing or use of high quantity of dye at the time of dyeing process. Moreover, the present procedures are not only time consuming and high cost but also produce higher quantity of waste in the textile industry. While attempts have been made over the years to attend to such problems most of the work had been tried to find out the right solution of colour deepening of the synthetic fiber but none of the attempted works fulfill the need to tackle all problems raised during synthetic fabric or fiber dyeing. Dyeing of synthetic fabric or fiber is not only problem but thermal migration is also an additional problem after dyeing the synthetic fabric or fiber.
In the publication of "Dyes and Chemicals" Vol. 15, No 1, pages 3-8 (1970) the deepening effect in the synthetic fabric is stated to be achieved if refractive index of the fabric is reduced by way of chemical treatment. We have also learned that dyed, fabric treated with resin increase the deepening effect and reason for that colour deepening effect explained in "Fiber Engineering" Vol. 26, No. 3, page 188. It is learned that enhancement of colouring effect by reducing the reflection of the surface layer and as a result of increasing the light that is transmitted into interiors of fibers. Therefore, dyeing of polyester fibers or fabrics with disperse dye coated with a layer having low refractive index polymer like a low polymer of trifluorochloroethylene (refractive index 1.4) showed colour deepening. Japanese Patent Application Laid-open specification no 26232/80 disclosed a high bath concentrated dipping treatment is carried out at high temperature for uniform coating. The process however involves high quantity of mass to be heated up with a huge amount of energy requirement and the spraying also, is a complex and troubles some process. Moreover, the need for uniform coating is not addressed and
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thus a serious risk factor is there for getting a heterogeneous and uneven deepening effect formed after resin treatment.
US Patent 4,373,043, dt Feb. 8, 1983, by Wakayama Kazubisa Yagi and et. al. disclosed an emulsion for colour deepening on synthetic fiber and follows the concept to use resin having low refractive index. Wakayama formulated the emulsion by using an emulsion crosslinked polyurethane thermosetting resin and an emulsion of silicone resin. Wakayama also teaches the deepening effect of the emulsion on black fabric and none of the examples or embodiments explain- the effect on the other colour of the synthetic fabric. Importantly, Wakayama only discusses the value of L but doesnot mention-other two 'a' and 'b' values ((Lightness was expressed as dark to light with 0=black and 100=white. Green to red was expressed by the "a" value. A more positive value represented red, while a more negative value represented green (-80=green, 100=red). Blue to yellow was expressed by the "b" value. A more positive value represented yellow and a more negative value represented blue)). However, during the expression of colour deepening, expression of L,a, b are important to clearly understand the change in colour. In the black colour, a redish shade is appear after deepening and this red shade makes the fabric more dull but if a bluish tone appears after deepening, fabric or fiber looks more bright and deep black. It is the main requirement when synthetic fabric is dyed to black colour. So, expression of deepening value only by L value is found to be not a complete data to give the real deepening effect after dyeing.
US patent 4,891,398. Dt 2nd January 1990 by Tanaka Masaki and et. al. discloses a fibre treatment composition comprising an aqueous dispersion containing a finely particulate epoxy organosilasesquioxane and a amono group containing organosiloxane. This composition is useful for deepening the colour of dyed textiles and improving the softness of the fabric. The invention also mentions colour deepening effect only with L value but doesnot disclose the effect on other colour value like "a" and "b". Thus while colour deepening is addressed by this prior art there is no clear direction to take care of any accompanying changing of the colour shade. More specifically, while the colour deepening values achieved for black fabric or fibres are provided the deepening effect in other dyed colour fibre and fabrics remain undisclosed.
Also, in all the above prior art developments regarding colour deepening emulsions, another important parameter after dyeing of the fabric is not addressed. This is concerning the fact that normally, in the synthetic fibre, there are no reacting group those can react with the dye and specially, in case of polyester, disperse dye is used which is embedded in the fibre at high temperature when the fibre become sift at high
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temperature. After cooling the fibre or fabric, most of dyes are loosely embedded on the fibre or fabric and later stage, when these fibre or fabrics are washed with detergent, gradually these dyes go off and fabrics or fibres become dull and ugly due to lose of dyes.
Considering the drawbacks of the above prevailing state of the art as described above, there is an urgent necessity to develop a formulation that gives good deepening effect without changing the colour shade of the fibre or fabric. In addition to this, there is the need that such formulation also imparts excellent softness in the fibre or fabric. Simultaneously, the formulation is required to protect the colour for required maintenance of the colour /dye during wash/use cycles.
OBJECTS OF THE INVENTION
It is thus the basic object of the present invention to develop a formulation that would be adapted to develop a significant colour deepening effect after treatment on fibre or fabric without changing the colour shad of the fibre or fabric.
Another object of the present invention is to develop a formulation that would favour very good durable softening effect in fibre or fabric after treatment with the formulation.
A further object of the present invention is to develop a formulation that would resist migration of dye during washing with detergent by way of fine flexible permanent coating on the dye.
Yet further object of the present invention is to develop a formulation that can be readily used in the textile industry in all possible finishing machines and no special system would be required for the application and use of such emulsion formulation. Another object of the present invention is directed to an emulsion formulation which would be simple and cost-effective to obtain and use for wide scale favourable use and application in the textile industry.
SUMMARY OF THE INVENTION
According.to the above discussed basic objectives of the present invention, there is to provided a fibre or fabric treatment composition adapted to impart colour deepening effect on dyed synthetic fibre and fabric together with a very good soft hand. Deepening effect of the formulation of the invention is found to be so unique that it is not only
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deepening the colour of the dyed fabric but also prevents the development of any undesirable colour alongwith desired colour formation. According to the present invention, the composition also helps to resist the migration of colour when washed with detergent.
Thus according to the basic aspect of the present invention there is provided a fibre or fabric treatment composition/emulsion comprising
(i) selectively a powder or liquid or solvent solution of organopolysiloxane resin having the following general unit formula (I)
Rl SiO (2n+l)/(n+l) (I)
Where R1 is a selected from a group consisting of monovalent hydrocarbon groups consisting 1 to 10 carbon atoms, "n" is an integer and varies from 1 to 5.
(ii) selectively a liquid of a specific amino functional organopolysiloxane having the following unit formula (ii)
(R2)a(W)b SiO (4-a-b)/2 :(II)
Wherein R2 is selected from a monovalent hydrocarbon group having 1 to 8 carbon atom or may be substitute by a group represented by the formula D OR3 where R3 is an alkyl group having 1 to 4 carbon atom, "a" & "b" are the integers and "a" values varies from 1 to 3 and "b" varies from 0 to 1. W is the amino functional group is repented by the following unit formula
R6
ID R4NR5 (Ill)
Where R4 is divalent hydrocarbon having carbon chain length 1 to 6. R5 and R6 may be same or different and each are a hydrogen atom or a monovalent hydrocarbon group having 1 to 8 carbon atoms.
Amino functional organopolysiloxane having unit formula (II) and with control of amine group as per formula (III) is design in a manner so that amine number of amino fluid is not more than 0.2.( amino number is expressed in term of milligram of KOH/gm of organopolysiloxane); and
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(iii) an non-ionic emulsifier/s use to make the emulsion of structure (I) and (II).
in accordance with a preferred aspect of the present invention there is provided a fibre or fabric treatment composition/emulsion comprising
(i) 100% powder or liquid or solvent solution of organopolysiloxane resin having the following general unit formula (I)
R1 SlO (2n+l)/(n+l) (I)
Where Ri is a selected from a group consisting of monovalent hydrocarbon groups consisting 1 to 10 carbon atoms, "n" is an integer and varies from 1 to 5. (ii). 100% liquid of a specific amino functional organopolysiloxane having the following unit formula (ii)
(R2)a(W)b SiO (4.a.b)/2 (II)
Wherein R2 is selected from a monovalent hydrocarbon group having 1 to 8 carbon atom or may be substitute by a group represented by the formula ? OR3 where R3 is an alkyl group having 1 to 4 carbon atom, "a" & "b" are the integers and "a" values varies from 1 to 3 and "b" varies from 0 to 1. W is the amino functional group is repented by the following unit formula
R6
I
? R4NR5 (Ill)
Where R4 is divalent hydrocarbon having carbon chain length 1 to 6. R5 and R6 may be same or different and each are a hydrohen atom or a monovalent hydrocarbon group having 1 to 8 carbon atoms.
Amino functional organopolysiloxane having unit formula (II) and with control of amine group as per formula (III) is design in a manner so that amine number of amino fluid is not more than 0.2.( amino number is expressed in term of milligram of KOH/gm of organopolysiloxane).
(iii) An non-ionic emulsifier/s use to make the emulsion of structure (I) and (II). The Non-ionic emulsifier/s used to make emulsion must be free from alkyene oxide groups that normally present in the non-ionic emulsifiers. Non alkylene oxide based non-ionic surfactant, specially, sugar derivatives capped with fatty alcohol or fattyl
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acid having HLB value (Hydrophilic Lyophilic Balance) from 9 to 19 is suitable for stable emulsion. Alkyl group present in fatty alcohol or fatty acid having carbon chain length varies from 8 to 30 are giving optimum stability in the final emulsion. Non ionic surfactant used for the emulsification of structure (I) and (II) together has a dual role. Sugar based non-ionic surfactant is not only helps to make the stable emulsion but also have important role for imparting optimum deepening effect on the dyed fibre or fabric.
In accordance with a preferred aspect of the present invention the above fibre or fabric treatment composition/emulsion comprises of biocide to resist the emulsion from microbial contamination. Generally, formalin, Kathon LXE, 2-phenoxy ethanol are found suitable for the this novel emulsion. Biocide quantity in-between 0.1 to 5% and most preferably 1 to 4% shows an average microbial stability more than one year.
According to a further preferred aspect of the invention the fibre or fabric treatment
composition/emulsion comprises
an additional softening effect on the treated fabric comprising an aqueous dispersion
containing
i. 5 to 25% resin having unit structural formulation (I)
ii. 10 to 30 % Amino functional organopolysiloxane having unit
structural formula (II) iii. 3 to 20% sugar based non ionic emulsifier/s having HLB value 9 to
19.
iv. 0.1 to 5% biocide. v. Rest is water.
According to yet further aspect of the present invention there is provided a process for the manufacture of the fibre or fabric treatment composition/emulsion comprising the steps of :
(a) Take (i) & (ii) in tank and mix till a uniform mixture is formed.
Add (iii) and 2% to 8% water. Homogenise the mixture till a uniform
paste is formed.
(b)Dilute the emulsion gradually with water and mix the water
through homogenise after each addition of water.
(c ) Add (iv) in the emulsion and mix by homogeniser.
The above composition of this invention can be applied on textile, especially on synthetic dyed fibre or fabric for achieving colour deepening effect without any development of
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undesirable colour after development of desire colour deepening. This composition of the invention is found to achieve an unique and long lasting softening effect on the treated textile and develop a high resistant of dye migration during the wash with non-ionic detergent.
DETAILED DESCRIPTION OF THE INVENTION
According to the present invention, the component of organopolysiloxane resin with a unit structure (I) where R1 is a mono hydrocarbon group consisting 1 to 10 carbon atom and this hydrocarbon group may include, for example methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tertbutyl, n-pentyl, Isopentyl, neopentyl, tertpentyl, hexyl such as n-hexyl, heptyl, such as n-heptyl, octyl, such as n-octyl and isooctyl, such as 2,2,4-trimethyl pentyl, nonyi, such as n- nonyl, decyl such as n decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecyl; alkenyl, such as vinyl and allyl, cycloalkyl,.such as cyclopentyl, cyclohexyl, cycloheptyl and methyl cyclohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, such as benzyl, a and b-phenylathyl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred.
Resin used in the-present invention is a mixture of trifunctional silicone unit and tetrafunctional silicone unit or only with trifunctional silicone unit or only tetrafunctional silicone unit. Silicone resin used in the present invention has unique properties and is remarkably reduced the gloss of the fabric and form a unique thin coating on the fibre. Therefore, a flexible structure is necessary to achieve a flexible coating. This flexible coating is necessary to protect the dye entrapped on the fibre surface. Generally, if only tetrafunctional silicone is used, final coating become brittle and dye can be migrated during washing from the treated fabric. Therefore, in the resin structure a composition of tetrafunctional and trifunctional silicone or only trifunction silicone is most preferable.
According to the present invention, the component of amino functional organopolysiloxane having unit structure (II) wherein R2 is a monovalent hydrocarbon group consisting 1 to 10 carbon atom.and this hydrocarbon group may include, for example methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tertbutyl, n-pentyl, Isopentyl, neopentyl, tertpentyl, hexyl such as n-hexyl, heptyl, such as n-heptyl, octyl, such as n-octyl and isooctyl, such as 2,2,4-trimethyl pentyl, nonyl, such as n- nonyl, decyl such as n decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecyl; alkenyl, such as vinyl and allyl, cycloalkyl, such as cyclopentyl, cyclohexyl, cycloheptyl and methyl cyclohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl,
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such as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, such as benzyl, a and b-phenylathyl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred.
According to the present invention, the component of amino functional organopolysiloxane having structure (III) wherein R4 is selected from a divalent hydrocarbon group having 1 to 10 carbon atom and this hydrocarbon group may include, for example methylene, ethylene, propylene, iso propylene, butylene, Isobutylene, pentylene,Isopentylene, neopentylene,
hexylene, heptylene, octylene,nonylene,decylene of which methyene,
ethylene,propylene, iso butylene are preferred and propylene is particularly preferred.
R5 and R6 in amino organosiloxane (III) may be same or different and each are a hydrohen atom or a monovalent hydrocarbon group having 1 to 10 carbon atoms and this hydrocarbon group may include for example methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tertbutyl, n-pentyl, Isopentyl, neopentyl, tertpentyl, hexyl such as n-hexyl, heptyl, such as n-heptyl, octyl, such as n-octyl and isooctyl, such as 2,2,4-trimethyl pentyl, nonyl, such as n- nonyl, decyl such as n decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecyl; alkenyl, such as vinyl and allyl, cycloalkyl, such as cyclopentyl, cyclohexyl, cycloheptyl and methyl cyclohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, such as benzyl, a and b-phenylathyl, of which hydrogen, methyl, ethyl, n-propyl, isopropyl are preferred and hydrogen is particularly preferred.
According to the present invention, amino organosiloxane has an important role to achieve desire colour deepening effect and uniform coating by way of uniform cross linking in-between resin and amino organopolysiloxane. Amino organopolysiloxane is also imparting excellent soft feel in the finished fabric. Gemerally, amino group always develop colour deviation of the dyed fabric and normally, it is one of the big negative of amino organopolysiloxane. This tendency of the colour change is also dependent on the type of amino group present in organopolysiloxane. It has been found that mono amine containing
Functional group has least color changing tendency in respect to di or tri or so on. There are also another way to control the less degree of colour change is to reduce the amine number of the product. It is well known art that an amino organopolysiloane having amine number less than 0.15, has a less tendency to react on the fabric dye. Considering the above mechanism, it is clear that amino organopolysiloxane. having monoamine functionality with amine number less than 0.15 shows almost no change in
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colour tone. Since amino group has a very high reactivity towards silicone resin, it is an objective to crosslinked resin with amino organopolysiloxane in a homogenous way or uniform way mean an uniform reaction takes place when amino polysiloxane and silicone resin come in contact with each other. This uniform crosslinking also helps to develop a stable flexible coating on the fibre. High amine number amino fluid and amino functionality more than one amine has a tendency to go for heterogeneous crosslinking system and resultant flim become more non-uniform and brittle. Hence, fiber treated with heterogeneous crosslinked polymer can not resist dye migration during washing due to its brittle configuration. The ratio of amino organopolysiloane to silicone resin in the final formulation also has an important to control the low refractive index in the final crosslinked film. Generally 2 part amino organopolysiloxane with 0.5 to 2 part silicone resin composition shows good colour deepening effect. More particularly, 2 part amino organopolysiloxane with 0.8 to 1.2 part silicone resin composition shows good optimum colour deepening effect.
According to the present invention, surfactant used for emulsification of an amino organopolysiloxane and silicone resin is critical not only for the stability of the emulsion but also optimized the colour deepening effect. All alkyl phenol ethoxylate like nonyl phenol ethoxylate, octyl phenol ethoxy and so on but not limited to only the said groups, are hindering the colour deepening effect and the similar hindering effect is also observed in case of fatty acid or fatty alcohol ethoxylate like lauryl alcohol ethoxylate, tridecyl alcohol ethoxylate, strearic acid ethoxylate, lauric acid ethoxylate and so on but it is not limited to said groups only. It is observed that sugar derivative of fatty alcohol like lauryl alcohol, tridecyl alcohol, Amyl alcohol, Stearyl alcohol and so on or fatty acid like lauryl acid, tridecyl acid, Amyl acid, Stearyl acid and so on, shows optimum result in consideration of stability of the emulsion and no hindrance on colour deepening effect. HLB value of the sugar derivatives having HLB value 9 to 19 shows good stability of the emulsion and most preferably, HLB value 10 to 15 gives optimum effect both in stability of the emulsion and no hindrance of deepening effect in the treated fabric. Generally 3 to 20% emulsifier is used to make the stable emulsion and most preferably, 4 to 10 % gives best stability and deepening effect in the treated fabric.
An addition of biocide is important to resist the emulsion from microbial contamination, is very much important. Generally, formalin, Kathon LXE, 2-phenoxy ethanol are found suitable for the this novel emulsion. Biocide quantity in-between 0.1 to 5% and most preferably 1 to 4% shows an average microbial stability more than one year.
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Therefore, the present invention provides a fibre or fabric treatment composition superior in colour deepening effect without developing any un-desirable colour and resist dye migration from the dyed fabric by way of a simple treatment of emulsion in the fibre or fabric preferably with an additional softening effect on the treated fabric .
In accordance with an aspect the fabric/fibre treatment composition comprises an
aqueous dispersion containing
(i) 5 to 25% resin having unit structural formulation (I) (ii)10 to 30 % Amino functional organopolysiloxane having unit structural formula (II)
(iii)3 to 20% sugar based non ionic emulsifier/s having HLB value 9 to 19, most preferably use 4 to 10% with preferable HLB value 10 to 15.
vi. 0.1 to 5% biocide,most preferably use 1 to 4%. vii. Rest being water.
The process for obtaining the above treatment formulation according to an aspect can
comprise:
(a) Take (i) & (ii) in tank so that the ratio of (i) and (ii) lies in-between 2: 0.5 to 2 and more preferably 2: 0.8 to 1.2 and mix the two components till a uniform mixture formed
(b)Add (iii) and 2% to 8% water. Homogenise the mixture till a uniform paste is formed.
(c )Dilute the emulsion gradually with water and mix the water through homogenise after each addition of water, (d )Add (iv) in the emulsion and mix by homogeniser.
The above composition of this invention can be applied on textile, especially on synthetic dyed fibre or fabric for achieving colour deepening effect without any development of undesirable colour after development of desire colour deepening. This composition of the invention also showed an unique and long lasting softening effect on the treated textile and develop a high resistant of dye migration during the wash with non-ionic detergent.
The details of the invention, its objects and advantages are explained hereunder in greater detail in relation to non-limiting exemplary illustrations as per the following examples:
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Examples
i) Comparative example 1 - Preparation of aqueous organosilasesuioxane dispersion
The known process for obtaining the dispersion followed was as per process laid down in Patent US 4,891,398. A mixture of 180 gm methyltrimethoxysilane with 20 gm of glycidoxypropyltrimethoxysilane, 20 gm of a cationic surface active agent lauryl trimethyl ammonium chloride, 20 gm of a non-ionic surface active agent polyxyethylene nonyl phenyl ether (HLB 18.5) and 658 gm water were emulsified with the use of homogeniser and emulsion was charged into a flask having 2 lit capacity and equipped with a stirrer, thermometer and reflux condenser. A solution made by dissolving 2 gm of sodium hydroxide in 100 gm water was added in the flask. Emulsion temperature Increased to 50°C so that no gellation formed during the reaction. Finally emulsion was cooled to 30°C. Finally measured the particle size and found 72 nm.
ii) Comparative example 2- Preparation of aqueous dispersion of amino group containing organopolysiloxane.
For such purpose a known similar dispersion as per process laid down in Patent US 4,891,398 was followed. An amino fluid was made as per description made in example 2 in US 4,89 Viscosity of the final fluid was 770 Cps and 4 no aminoethylamino propyl group present in one molecule of the polymer. Amine number of the fluid was 0.52.
15 part of the above amino fluid, 2 part polyoxyethylene alkyl phenol ether and 83 part water were added, followed by stirring and used homogenizer to make the emulsion.
iii) Comparative example 3 - Preparation of Comparative fibre treatment composition
For such purpose again a known similar composition as per patent US 4,891,398 was followed for the fibre treatment from the above comparative example 1 & 2 with following the guideline from the said patent that showed the best performance in application. The test dispersion was made after mixing 2 part comparative emulsion 2 and 1 part comparative emulsion 1.
Further test formulations were obtained as further detailed hereunder:
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Example A -
An methyl resin was made by hydrolysis of methyl triethoxy silane and tetraethyl orthosilicate in a ratio of 50:50. Controlled hydrolysis was done at 15-20°C by water at pH 10 and after hydrolysis, neutralised the resin by acetic acid. Increased the material temperature to 70°C and removed the alcohol by vacuum.
Made an amino fluid having amine number 0.3 with polymer construction alpha ,omega trimethylsiloxymethylpolysiloxane with an aminopropyl functionality in the branch. Viscosity of the polymer was 1100 mPas having average molecular weight 15400. Fluid made by taking octamethylcyclotetrasiloxane, Aminopropylmethyldiethoxysilane and hexamethyldisiloxane in the ratio of 94:4:2 at 140°C by using 25ppm KOH for 4 hr. Neutralise the fluid with acetic acid. Distil the fluid at 170°C under vacuum.
An emulsion made by taking the above Amino fluid and methyl resin in a percentage of 20% and 10% and mix till a uniform mixture developed. Added 6% Lauryl alcohol capped glucose derivative having HLB value 13 and 4% water. Homogenised the mixture till a uniform paste was developed, gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
Example B -
Made an amino fluid having amine number 0.3 with polymer construction alpha, omega trimethylsiloxymethylpolysiloxane with an aminopropyl functionality in the branch with a trifunctionality. Viscosity of the polymer is 1200 mPas having average molecular weight 16500. Process was same like example A with a ratio of 92:4.5:3.5 of octamethylcyclotetrasiloxane, Aminopropyltriethoxysilane and hexamethyldisiloxane
An emulsion made by taking the above Amino fluid and methyl resin from example A in a percentage of 20% and 10% and mix till a uniform mixture developed. Added 6% Lauryl alcohol capped glucose derivative having HLB value 13 and 4% water. Homogenised the mixture till a uniform paste was developed, gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
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Example C-
An methyl resin was made by hydrolysis of 100%
methyl triethoxy silane . Process was same like Example A.
An emulsion made by taking the same amino fluid from example A
and methyl resin from above in a percentage of 20% and 10% and mix till a uniform
mixture developed. Added 6% Lauryl alcohol capped glucose derivative having HLB
value 13 and 4% water. Homogenised the mixture till a uniform paste was developed.
gradually added 57% water in a number of steps with uniform mixing after each addition
of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a
biocide.
Example D-
Made an amino fluid having amine number 0.3 with polymer construction alpha, omega trimethylsiloxymethylpolysiloxane with an aminoethylaminopropyl functionality in the branch. Viscosity of the polymer is
1150 mPas having average molecular weight 14700. Process was same like example A
with a ratio of 92:4:4 of octamethylcyclotetrasiloxane,
Aminoethylaminopropylmethyldimethoxysilane and hexamethyldisiloxane
An emulsion made by taking the above Amino fluid and methyl resin from example A in a percentage of 20% and 10% and mix till a uniform mixture developed. Added 6% Lauryl alcohol capped glucose derivative having HLB value 13 and 4% water. Homogenised the mixture till a uniform paste was developed, gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
Example E -
An emulsion made by using same amino fluid and resin from example A in a percentage of 20% and 10% and mix till a uniform mixture developed. Added 6% isotridecylalcoholethoxylate 10EO HLB and 4% water. Homogenised the mixture till a uniform paste was developed, gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
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Example F-
An emulsion made by using same amino fluid and resin from example A in a percentage of 20% and 10% and mix till a uniform mixture developed. Added 6% Nonylphenolethoxylate 10EO and 4% water. Homogenised the mixture till a uniform paste was developed. Gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
Example G -
An emulsion made by using same resin from example A
in a percentage of 30% and added 6% Lauryl alcohol capped glucose derivative having HLB value 13 and 4% water. Homogenised the mixture till a uniform paste was developed, gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
Example H-
An emulsion made by using same amino from example A
in a percentage of 30% and added 6% Lauryl alcohol capped glucose derivative having HLB value 13 and 4% water. Homogenised the mixture till a uniform paste was developed. Gradually added 57% water in a number of steps with uniform mixing after each addition of water. pH was adjusted to 5 by acetic acid. Finally Added 3% 2 phenoxy ethanol as a biocide.
Using above composition from experiment A to H and comparative example 3, a black colour, violet colour and green colour polyester georgettes were treated in the following manner. For all tests, made
test solution by dissolving 40 gm emulsion in one litre water. For each test solution, above three colour fabrics dipped in the test solution and padded at 2 Kg nipped pressure with a 50% wet pick up in the fabric. Dried the fabric at 180°C for 1 hr. Conditioned the fabric at 80% RH for 4 hr. Then used thses fabric for the evaluation of colour deepening, softness and resistant to dye migration.
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Colour Deepening
Colour tone variation was measured by Hunter Lab ColorFex Spectrophotometer. We measured the L,a,b value of all the fabrics and the results are showed in table 1.
Table -1
Test fabrics Resin type Amine type emulsifier used L a b
Untreated Black 20.35 0.01 -2.29
Comparative example iii Epoxy,T AEAPD EO 18.37 5.03 0.03
Example A T/Q APD NON EO 16.92 -0.09 -4.04
Example B T/Q APT NON EO 16.55 -0.03 -3.98
Example C T APD NON EO 17.37 -0.05 -2.92
Example D T/Q AEAPD NON EO 18.6 4.78 0.07
Example E T/Q APD EO 18.67 0.03 -0.12
Example F T/Q APD EO ' 18.4 0.02 -0.05
Example G T/Q NON EO 19.90 0.01 -1.97
Example H APD NON EO 19.7 0.01 -1.34
Untreated Green 29.40 -2.5 3.4
Comparative example iii Epoxy,T AEAPD EO 29.3 -2.2 3.97
Example A T/Q APD NON EO 26.30 -4.03 3.2
Example B T/Q APT NON EO 26.8 -4.52 3.17
Example C T APD NON EO 26.88 -3.98 2.89
Example D T/Q AEAPD NON EO 28.97 -2.33 4.2
Example E T/Q APD EO 29.1 -2.2 3.22
Example F T/Q APD EO 29.3 -2.98 3.98
Example G T/Q NON EO 29.1 -2.54 2.78
Example H APD NON EO 29.23 -2.32 2.88
Untreated Violet 23.87 20.89 -26.02
Comparative example iii Epoxy,T AEAPD EO 22.96 20.45 -25.98
Example A T/Q APD NON EO 21.52 22.4 -27.76
Example B T/Q APT NON EO 21.34 22.98 -27.98
Example C T APD NON EO 21.78 22.67 -27.54
Example D T/Q AEAPD NON EO 22.78 20.2 -25.86
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Example E T/Q APD EO 23.2 19.87 -25.55
Example F T/Q APD EO 22.69 20.54 -25.21
Example G T/Q NON EO 23.54 20.78 -26.78
Example H APD NON EO 22.12 19.45 -22.1
L = 100 White a = more positive = Red b= more positive = Yellow
L = 0 Black a= more negative = Green b = more negative = Blue
Q - tetra functional; T - tri functional; AP - amino propyl; AEAP - amino ethylamino
propyl; EO - ethyleneoxide based surfactant; NONEO - non ethylene oxide based
surfactant.
From Table 1, it is clear that comparative example iii showed black deepening but the deepening effect is not in other colour. In the black also, though, fabric become more black but a distinct red colour appeared on the black colour. This is strictly undesirable for black colour.
On the other hand, colour deepening effect with Experiment solution A, B and C showed excellent deepening effect in all three colours without any side colour development.
Experiment D also showed aminoethylaminopropyl based amino functionality is also not suitable for colour deepening and developed side colour in black fabric. This amino functionality is also not suitable for other colour.
Experiment E & F also showed EO based emulsifiers also had problem in colour deepening effect.
Experiemnt G &H showed resin and amino fluid needed together to achieve the desire deepening effect and individually, non of the component showed any remarkable effect in the colour deepening.
Softness
Evaluation of the softness with four member panellist those experienced in evaluation of fabric softener for long time were asked to give point 5 for excellent and 1 for no effect. Since formulations of Examples A,B and C
showed good deepening effect, only these emulsion treated fabrics were considered in together with comparative emulsion treated fabrics for softness evaluation
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Table 2
Panellist Comparativ Experiment A Experiment B Experiment C
e emulsion treated treated treated fabric
treated Fabric Fabric
fabrics
B G V B G V B G V B G V
PI 3 3 3 4 4 5 4 4 3 4 4 5
P2 3 2 3 4 4 4 3 4 5 3 4 4
P3 2 2 3 3 4 3 4 4 4 3 4 4
P4 3 3 3 4 4 5 5 4 3 4 4 3
Av. 2 2. 3 3.75 4 4.25 4 4 3.7 3.5 4 4
Rating . 5
7
B - Black; G - Green; V- Violet.
From the softness evaluation data as in Table 2, it is cleared that softness wise, there were not much different in experiments A, B and C. But Comparative emulsion iii showed lesser softness compare to experiment A,B and C.
Colour migration Test.
Dyed the raw polyester fabric with Feron blueSE-2RI at 130°C under 4 Kg/cm2 pressure for 1 hr with a 2% dye pick on dry to dry basis. Then washed the fabric till the loose dye rinsed off totally.Dried the fabric till the water dried out from the fabric. Cut out four pieces of fabrics from the newly dyed fabric and treated separately with 40 gpl (gm per litre) solution of Experiment A, B, C and comparative emulsion iii. Cut out 100 gm of each dyed (without softener treated) fabric, comparative emulsion iii treated fabric, Experiment A emulsion treated fabric, Experiment B emulsion treated fabric and Experiment C emulsion treated fabric. Took five 2 lit beaker and put the fabric each fabric separately in five 2 lit beaker. Poured 2 Kg monoethyleneglycol and kept for 2 hr for extraction of dye by monoethylene glycol. Measured the dye quantity in monoethylene glycol by UV spectrophotometer. Results of the percentage of dye migration is tabulated in table 4.
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Table 3.
Migration Rating of Disperse Dyes Based on the Migration Test.
Dye retained after washed with Migration Rating
monethylene glycol
Below 50 6
55-50 5
60-55 4.5
65-60 4.0
70-65 3.5
75-70 3.0
80-75 2.5
85 -80 2.0
90-85 1.5
95-90 1.0
Table 4
Fabric Identification Blank fabric dye wt, gm Dye lost by washing with MEG, gm % of retained Dye Migration rating
only dyed fabric 2.12 1.13 46.7 6
Fabric treated Exp A Emul. with 2.12 0.85 60 4.5
Fabric treated Exp B Emul. with 2.12 0.27 90 1.5
Fabric treated Exp C Emul. with 2.12 0.21 91 1.0
Fabric treated comparison emul with . iii 2.12 0.24 88.6 1.5
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From the above table 4, it is clear that the emulsions of Examples A, B and C are not only excellent to develop excellent desired colour deepening effect but also impart very good softness and remarkably resist the dye migration during washing.