FIELD OF THE INVENTION
The present invention relates to a formulation for softening and lubrication of lignocelluiosic fibers such as Jute, Mesta and allied fibers and, in particular, to a stable organopolysiloxane emulsion / bath liquor useful for such lubrication and softening of lignocelluiosic fibers and the like. Importantly, the organopolysiloxane emulsion / bath liquor of the invention avoids the use of the conventional mineral oil (JBO or Jute Batching Oil) used for such lubrication and softening of jute fibers and is provided absolutely free from typical organic oils or mixture of organic oils and thereby favour obtaining of jute / Hessian and other lignocelluiosic fiber based products free of any harmful organic contaminants. Moreover, the organopolysiloxane emulsion based lubricant and softener is free of any obnoxious, avoids transfer of non-hygienic organics into food grains during storage of such in jute and Hessian sacks and is absolutely non-toxic, inert and highly stable in wide range of temperature for wide scale application and use for variety of lignocellulosic/jute products. The organopolysiloxane emulsion is thus directed to replace organic oil completely in the processing of lignocellulosic / jute fiber and would favour cost effective and user friendly processing of fibers wherein spinning time would be significantly reduced with minimum of fiber breakage as compared to organic / mineral oil based lubricants / softeners presently in use. The invention involving the organopolysiloxane emulsion would thus favour increasing productivity maintaining desired fiber characteristics such as tensile strength, quality ratio, strength CVetc.
BACKGROUND ART
It is well-known that lignocelluiosic fibers such as jute fiber consist of cellulose (58-83%), hemi celluloses (21-24%), lignin hemi celluloses which act as the cementing materials (12-14%), wax (0.4-0.8%), pectin (0.2%-0.5%). It is also known that due to the presence of high amount of hemi cellulose and lignin in jute it is very harsh and rigid. Jute readily absorbs water and swells thereby causing the fail in wet strength of the fiber. It is, therefore, essential that jute and allied fiber are softened with proper lubrication before subjecting to any carding and drawing to convert jute fibre into spinable form.
Jute Batching Oil (JBO) is basically a mineral oil with boiling range between 240 to 400°C and is commercially used for lubricating and softening of jute fibres. Such JBO is found to suffer from some inherent disadvantages for use as a lubricant / softener for jute and allied fibre because in the lower part of its boiling range, a kerosene smell predominates, while at the higher part of the boiling range it smells of cracked petroleum, a of fishy
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odor. Moreover, it is also found to contain undesirable constituent like pyrene and polynuclear aromatic hydrocarbon, which are found to be carcinogenic (as per ISI specification). Such inherent concerns of JBO is found to affect its use in jute and allied fibre processing using such mineral oil / JBO since the fibre processed involving such JBO are found to be contaminated with harmful and health hazardous constituents of the mineral oil. The demand for jute and allied fibres and products thereof free of any mineral oil / hydrocarbon contamination has been generated keeping in view such problems associated with processing of jute fibre using the conventional JBO. This has lead to developments directed to possible suitable substitutes for JBO as a lubricant/softener and more Importantly to get an alternative lubricant/softener free from such hydrocarbons contamination.
IN 173586 discloses a composition for softening cum lubrication of jute fibres as additive to jute batching oil comprising of an anionic softener being a sufonated product of a non-edible oil such as castor oil, linseed oil, sal seed oil and like, and a swelling agent such as diammonium carbamide and diammoniuim sulphamide in the ratio of 4 to 5: 3 to 4 by weight. It would be apparent from the disclosure in IN 173586 that attempt was made to reduce the quantity of JBO with an additional use of sulfonated fatty oil like castor oil, linseed fatty oil, sal seed oil in the emulsion of JBO. The use of reduced amount of JBO was also directed to minimize bad odor of JBO and also harmful effects on the end product due to its processing involving wholly of JBO. However, the formulation

proposed continued to incorporate obnoxious smelling compound like sulfonated castor oil, linseed oil and sal seed oil.
IN 178368 discloses another composition suitable for use of softening and lubrication of lignoceliulosic fibres which basically comprised 2% to 5% by weight of non-edible vegetable oil, an anionic emulsifier in the ratio of 1:10 with respect to the said oil, 0.05% to 0.1% by weight with respect to the oil, of a preservative, and 0.5% to 2% by weight, of the total weight of the emulsion, of an anionic softener and the rest being water.
In this above prior art of IN 178368 instead of harmful JBO the use of non-edible vegetable oils like castor oil and cotton seed oil have been proposed. However, such alternative non-edible oil replacing JBO also are known to have strong bad smell which are ultimately transferred to yarn or the products obtained of fibres processed using such oils. Importantly also, vegetable oils have problems of rancidity, some oil rancid faster while some take time to rancid. Anyway, such vegetable rancid oils are again health hazardous and it is desirable to carry over of such oil contaminants to food grains
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and / or other fibre products obtained following processing of fibres involving such possible vegetable rancid oils. Added to the above, it is also relevant to add that presently organic oil prices are high and use of such oils proposed in the prior art make the processing of jute and allied fibres expensive. Its an another additional cost is its intensive processing in I jute industries, is to make emulsion of JBO/organic oil continuously prior to use in the application with an additional deployment of man power
It is thus apparent from the above state of art that while it is well known that JBO as a lubricant and softener for processing of jute and allied fibres is harmful and health hazardous there is a continuing need in the art to provide for effective alternative to JBO
which would serve on one hand as an effective lubricant and softener and on the other
hand would also not have the problem of JBO and other vegetable rancid oil and thereby
enable safe, healthy and also cost effective processing of jute and allied fibres for wide scale application and use of lignocellulosic fibre based products for variety of end use / applications including packaging of food grains and the like without any health concerns without increasing cost of production and easier to apply/process
OBJECTS OF THE INVENTION
It is thus the basic object of the present invention to provide a much required suitable alternative to mineral oils/JBO/organic oil for use as lubricant / softener for the processing of lignocellulosic fibres which would not have harmful carcinogenic nature of mineral oil and / or suffer from bad odor of JBO and other rancid vegetable oils and thereby favour processing of such fibres involving a safe and effective lubricant and softener composition.
Another object of the present invention is directed to the development of an organopolysiloxane emulsion based lubricant and softener formulation for processing of lignocellulosic based fibres such as Jute, Mesta and allied fibres which would on the one hand be simple and cost effective to obtain and on the other hand provide a simple and cost effective alternative to the harmful and hazardous JBO or organic oils presently in use for softening and lubrication of jute and allied fibres.
Another object of the present invention is directed to the development of an organopolysiloxane based emulsion for treatment of lignocellulosic / jute fibres which would be simple and cost effective and available in emulsion form and would not require -additional man and/or machine continuously to produce such emulsion but dilute the
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emulsion simply by water at a time for few days work based on the quantity of jute and allied fibres to be processed.
A further object of the present invention is directed to an organopolysiloxane emulsion based lubricating and softener formulation as an effective alternative to mineral oil / JBO which would not carry any kind of smell of the fibre processed and would also not be health hazardous and can be safely used to process fibre and produce products there from to safely store even food grains free of any hazardous / harmful contamination.
Yet further object of the present invention is directed to a stable organopolysiloxane emulsion based lubricating and softener formulation which after application in jute fibre and / or other allied fibre would not show any change in properties even under extreme temperature range, such as of -40®C to ° 150°C.
A further object of the present invention is directed to providing an organopolysiloxane emulsion based lubricating and softening composition for processing of lignocellulosic fibres such as jute fibres and the like, which would effective in low concentration of as low as 0.1% thereby making the process of softening of such fibres simple and importantly cost effective.
Yet further object of the present invention is directed to make the processing of lignocellulosic or jute and allied fibres simple and cost effective by significant reducing cost of chemicals / lubricants / softeners and also enabling faster productivity by way of faster spinability.
SUMMARY OF THE INVENTION
Thus according to the basic aspect of the present invention there is provided a stable organopolysiloxane emulsion/bath liquor for the lubrication and softening of lignocellulosic fibres such as jute and allied fibres having particle size up to 10 micron comprising:
(a) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt. (b) water in an amount of 20 to 75 % by wt. (c) selective non-ionic emulsifier(s) having HLB in the range of 10-19 in amounts of 1 to 15% by wt. and (d) selective anionic emulsifier having HLV in the range of 8 - 19 in an amount of 1 to 15 % by. Wt.
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The stable organopolysiloxane emulsion/bath liquor of the invention for use as lubricant and softener for lignocellulosic fibres also selectively comprises wetting agent/s preferably in a ratio of 1 part organopolysiloxane emulsion and 0.2 parts wetting agent/s to 1part organopolysiloxane emulsion and 0.5 part wetting agent/s and an organic fertilizer preferably with an inorganic control releasing agent favouring the organopolysiloxane penetration to root portion of raw jute fibre.
The organic fertilizer can comprises an amine based organic fertilizer preferably selected from urea and derivatives of urea and in amount of from 0.1% to 2.0% for the root processing and alkali metal salt in a small amount in the range of 0.01% to 1% selectively provided as control release agent for the organic fertilizer.
In the above disclosed stable organopolysiloxane emulsion/bath liquor the Low molecular organopolysiloxane is preferably selected form alpha omega hydroxy terminated organopolysiloxane; alpha omega alcoxy terminated organopolysiloxane; cydo organopolysiloxane or mixture thereof. In case of branched polysiloxane emulsion incorporating a tri functional or tetra functional silane or a mixture thereof in amounts from 0,1 to 5% depending on the degree of branching in siloxane molecule.
The Anionic surfactant is preferably selected from organic sulfonic acids, preferably selected from alkyl aryl sulfonic add; alkyl aryl polyoxyethylene sulphonic add; alkyl sulfonic add and alkyl polyoxyethylene sulfonic add.
According to an aspect the stable organopolysiloxane emulsion/bath liquor comprises of non ionic surfactant(s) having HLB value in-between 12-15 to get an emulsion of organopolysiloxane having long self life.
In accordance with yet another aspect of the present invention there is provided a process for softening and lubrication of lignocellulosic fibres such as jute and allied fibres comprising:
a) providing a final bath liquor comprising organopolysiloxane emulsion having particle size up to 10 micron in the range of 0.5 % to 10% comprising of (a) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt. (b) water in an amount of 20 to 75 % by wt. (c) selective non-ionic emulsifier(s) having HLB in the range of 10-19 in amounts of 1 to 15% by wt and (d) selective anionic emulsifier having HLV in the range of 8 - 19 in an amount of 1 tol5 % by. wt. and with addition of (i) wetting agent/s in a ratio of 1 part organopolysiloxane emulsion and 0.2 parts wetting agent/s to 1 part
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organopolysiloxane emulsion and 0.5 part wetting agent/s; and (ii) organic fertilizer from 0.1% to 2.0% with an inorganic control releasing agent with preferably alkali metal salt in a small amount in the range of 0.01% to 1% for improving the organopolysiloxane penetration to root portion of raw jute fibre; and (iii) rest portion made up with water; and
b) subjecting the lignocellulosic fibres, jute/allied fibres, to treatment in said bath liquor for the desired softening of the fibres.
In the above process for softening and lubrication of lignocellulosic fibres during jute processing, the said bath liquor is preferably applied 20-25% by weight depending on the grade of the jute.
DETAILED DECRIPTION OF THE INVENTION
The invention thus provides an use of organopolysiloxane emulsion having particle size up to 10 micron from a low molecular organopolysiloxane or a mixture of organopolysiloxane (henceforth refer as blended organopolysiloxane). Low molecular organopolysiloxane may be alpha omega hydroxy terminated organopolysiloxane; alpha omega alcoxy terminated organopolysiloxane; cycle organopolysiloxane or mixture thereof.
Preferably, add a tri functional or tetra functional or a mixture thereof in case of branched polysiloxane emulsion. Quantity of siiane can vary from 0.1 to 5% depending on the desire degree of branch in siloxane molecule. If branched polysiloxane is not needed, the siiane addition is avoided.
The alpha omega functional end blocked linear organopolysiloxane used herein are preferably those of the general formula I:

Where Rl hydrogen or a monovalent hydrocarbon group of 1 to 10 carbon atoms or a hydroxyl group or an alcoxy group having Ito 8 carbon atoms. Examples of Rl as a monovalent hydrocarbon groups are methyl, ethyl, n-propyl, isopropyl, n-butyl, Isobutyl, tert-butyl, n-pentyl, Isopentyl, neopentyl, tertpentyl, hexyl such as n-hexyl, heptyl ,
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such as n-heptyl, octyl, such as n-octyl and isooctyl, such as 2,2,4-trimethyl pentyl, nonyl, such as n- nonyi, decyl such as n decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecyl; alkenyl, such as vinyl and aliyf, cydoalkyl/ such as cyclopentyl, cydohexyl, cydoheptyi and methyl cydohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl xylyl and ethylphenyl; aralkyl, such as benzyl, a and ß-phenylathyl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred. Example of R1 as alcoxy groups are methoxy, ethoxy, propoxy, butoxy, pentoxy, nexoxy or a phenoxy group but not limited to the said groups.
Where R, which may differ, is a monovalent hydrocarbon radical. Examples of R are alkyl radicals, such as methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tertbutyl, n-pentyt, Isopentyl, neopentyt, 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, cydoalkyl, such as cydopentyl, cydohexyl, cydoheptyi and methyl cydohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl; alkylaryl, sudi as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, sudi as benzyl, a and ß -phenylathyl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred.
x is an integer from 1 to 100.
The organocydopolysiloxanes used herein have the following structure:

Where R is the independently hydrogen or monovalent hydrocarbon groups of 1 to 8 carbon atoms induding an alkyl group such methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tert-butyl, n-pentyl, Isopentyl, neopentyl, tert pentyl, hexyl such as n-hexyl, heptyl , such as n-heptyl, octyl, sudi 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 ailyl, cydoalkyl, such as cydopentyl, cydohexyl, cydoheptyi and methyl cydohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl, xylyl and ethylphenyl;
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aralkyl, such as benzyl, a and ß -phenylathyf, of which methyl, ethyl, n-propyl, isopropyl
are preferred and methyl is particularly preferred. 'n' is an integer of 1 to 8. Most
preferred organocydosiloxanes are octamethylcyclotetrasiloxane;
decamethylcydopentasiloxane; Oodecamethyl cydohexasiloxane; 1,2,3,4- tetramethyl-1,2,3,4-tetravinyl cydotetrasiloxane; 1,2,3,4- tetramethyl-l,2,3,4-tetraphenyl cydotetrasiloxane.
Organopolysiloxarne used according to the present invention may be branched by way of incorporation of branching units. Branching units may be introduced to improve the film forming behavior of organopolysiloxane. Branching unit may be trifunctional silane or tetrafuncbonal silane or a mixture thereof. Trifuntional silanes (HI) and tetrafunction silanes (IV) have the following structure:
R—Si — (O — R)3 m Si — (O — R)4 IV
Where R, which may differ, is a monovalent hydrocarbon radical. Examples of R are alkyl radicals, such as methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tert-butyl, n-pentyl, Isopentyl, neopentyl, tert pentyl, 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, cydoalkyl, such as cydopentyl, cyclohexyl, cydoheptyl and methyl cydohexyl, aryl such as phenyl, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, such as benzyl, a and ß -phenylathyl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred. Depending on the desired requirement of branching of the organopolysiloxane, branching units are adding during the emulsification process. 0.1 to 5% branching units of the emulsion is useful to make an emulsion containing organopolysiloxane having highly branched structure. Quantity use in the emulsion must be controlled carefully, otherwise gellation of the polymer may occur during emulsion process and emulsion become destabilizes.
According to the present invention, anionic emulsifier has an important role for stabilizing the emulsion and improves the penetration of organopolysiloxane into the raw jute fibre for attainment optimum softness and lubrication. Anionic surfactant is selected from organic sutfonic adds. Most common sulfonic adds used in the present process are alkyl aryl sulfonic add; alkyl aryl polyoxyethylene sulphonic add; alkyl sulfonic acid and alkyl polyoxyethylene sulfonic add. Structures of sulfonic adds are as below:

R2C6H4SO3H (V) R2C6H4O(C2H4O)mSO3H (VI)
R2SO3H (VI) R2O(C2H4O)mSO3H (Vm)
Where R2, which may differ, is a monovalent hydrocarbon radial having at least 6 carbon atoms. Most preferable R2 groups, but not limited to the following groups, are hexyl, octyl, decyl, dodecyl, cetyl, stearyl, myristyl, and oleyl. 'm' is an integer from 1 to 25. Most preferable anionic surfactants used in the present inventions are octyl benzene sulfonic add; dodecyl benzene sulfonic add; cetyl benzene suifonic acid; Alpha octyl sulfonic add; Alpha dodecyl sulfonic add; alpha cetyl sulfonic add; polyoxyethylene octyl benzene sulfonic add; polyoxyethylene dodecyl benzene sulfonic add; polyoxyethylene cetyl benzene sulfonic add; polyoxyethylene octyl sulfonic add; polyoxyethylene dodecyl sulfonic add and polyoxyethylene cetyl sulfonic add. Generally, 1 to 15% anionic surfactant is used in the present emulsion processing process. Preferably, 3- 10% anionic surfactant is used in the present emulsion to get the optimum result. Anionic surfactant has a dual role in the present emulsion process. Anionic surfactant acts as a condensation/ring opening catalyst in together with as a surfactant for emulsion making. Thus, by using anionic emulsifier, process doesnt need any additional catalyst for polymer growth of organopolysiloxane during emulsion process. According to the present invention, HLB value of the anionic emulsifier plays an important role for stabilizing the organopolysiloxane emulsion and penetrating potential of the emulsion in the raw jute fibre. Anionic emulsifier having HLB values 8-19 are found suitable to achieve the desire results. HLB value of the anionic emulsifier in-between 8-12 is most preferable to optimize the properties in the organopolysiloxane emulsion.
It is also observed according to the present invention, one additional emulsifier together with anionic emulsifier is preferred for making the emulsion more effective in the processing of raw jute fibre. It is spedally found by way of the present invention that at least one non-ionic emulsifier in together with anionic surfactant helps for faster penetration in the raw jute fibre. Non-ionic emulsifiers having HLB value in between 10-19 are suitable to make the emulsion more effective and stable. Most useful surfactants of this category are polyoxyalkylene alkyl ether, polyoxyalkylene alkylphenyl ethers and polyoxyalkylene sorbitan esters. Some useful surfactants having HLB value in between 10-19 are polyethylene glycol octyl ether; Polyethylene glycol lauryl ether; Polyethylene glycol tridecyl ether; Polyethylene glycol cetyl ether; Polyethylene glycol stearyl ether; polyethylene glycol nonylphenyl ether; polyethylene glycol dodecylphenyl ether; polyethylene glycol cetylphenyl ether; polyethylene glycol staerylphenyl ether; polyethylene glycol sorbitan mono stearate and polyethylene glycol sorbitan mono
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oleate. Non-ionic surfactant having HLB value in-between 10-19 has a great importance in the present invention to boost the emulsion penetration more faster in jute processing. Generally, 1 to 15% non ionic surfactant is used in the present emulsion processing process. Preferably, 3- 10% non ionic surfactant is used in the present emulsion to get the optimum result It is well known in the art that surfactant(s) have HLB value in-between 12-15 is useful to make organopolysiloxane emulsion by using simple shear mixer in shorter period and it is also well known to use a mixture of surfactants that have HLB value in-between 12-15 to get an emulsion of organopolysiloxane having long self life.
According to the present invention, organopolysiloxane emulsion having particle size up to 10 micro is found suitable for the processing the raw jute fibre. Particle size of the emulsion can be adjusted by changing organopolysiloxane to emulsifiers ratio and or by changing the ratio of anionic emulsifier and non ionic emulsifier. Organopolysiloxane emulsion having up to 1 micron is most preferable to achieve desire softness and lubrication of the jute fibre during processing.
According to the present invention, effective utilization of organopolysiloxane emulsion is depending on penetrating ability of the emulsion in raw jute. Due to wide variant and complex composition of jute, it is very difficult to penetrate fibre by organosiloxane emulsion with a definite amount of wetting agent in the emulsion though organopolysiloxane emulsion has high penetrating power due to low surface tension of the emulsion. Considering the wide fluctuation of feed quality, an additional quantity of anionic and non ionic emulsifiers in final bath liquor resolve the problem efficiently. Preferably, first, anionic to non-ionic is mixed in a ratio of 3:0.5 to 4:2 and most preferably 4:0.1 to 4:1.5. Mixed emulsifiers are used in the bath liquor in amounts of 0.1% to 5% and most preferably 0.3% to 0.6 %. Non-ionic and anionic emulsifiers are used similar type as described above but not limited to the said emulsifiers.
Importantly, according to present invention, addition of small amount of organic fertilizer in bath liquor helps organopolysiloxane to penetrate in root area. Urea or its derivative in a small quantity in the bath liquor shows remarkable effect by way of allowing organopolysiloxane penetration in the root area but effectiveness in organopolysiloxane in root area is not limited to this class of fertilizer only. Fertilizer from 0.1% to 2.0% is found effective in the root processing and 0.1% to 0-8% is preferred in this application. A control releasing additive is preferred to slow release of fertilizer from bath liquor for effective softening. Generally, an alkali metal salt like sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate and similar type of alkali metal salt in a small amount in the range of 0.01% to 1% is suitable for this application.
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Salt concentration in the range of 0-01% to 0-05% is preferable in this application and type of salt is not limited to the said class of compounds only.
In the final bath liquor, organopolysiloxane emulsion in the range of 0.5 % to 10% can be used together with surfactant mixture as discussed above and in addition to that, small quantity fertilizer and salt additive use as described above. Rest portion is made up with water. In the bath liquor, 1% to 3% of organopolysiloxane emulsion is preferably used to get an optimum processing properties.
During application, final bath liquor can be applied by any type of spraying system. Generally in the industry, liquor is spread over jute through drip feed on the softener machine and then jute bundles are passed through fluted rollers. Treated jute is staggered or piled for 24-72 hrs depending on the grade and humidity. Bath liquor is generally applied at 20-25% by weight depending on the grade of the jute. The actual application of organopolysiloxane is about 0.1% on the weight of the fibre.
After opening the piles, jute batches treated with organopolysiloxane liquor is processed through carding (Breaker card and Finisher card), drawing (1st drawing- finisher drawing) and spun into yarns.
EXAMPLES:
The organopolysiloxane emulsion for lubrication and softening of lignocellulosic fibres in accordance with the invention were obtained and further subjected to trials to ascertain its lubrication and softening characteristic vis-a-vis the convention JBO based softeners presently in use. The trials have been conducted on Hessian and sacking qualities and comparative studies were conducted by treating 150 tons jute and its performance in a pair of spinning frames and were observed for one week production. The results obtained are reproduced hereunder:
Organopofysiloxane Emulsion in accordance with the invention was obtained as per Examples I to X of Table 1 hereunder: TABLE - 1

Exam- Emuls. Organo. Viscosity of Particles size Anionic Non-ionic Organopolysi
pie Name polysiloxane organo- of the emulsifier emulsifier loxane
polysiloxane, emulsion content %
Cps.
I E1 Dimethiconol 25000 120 TEA Trideceth 30
LABS
II E2 Dimethiconol 80000 130
III E3 Dimethiconol 1000000 100
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IV E4 Dimethiconol 60000 105
V E5 Dimethiconol 10000000 125
VI E6 Vinyl Dimethicone 60000 130
vII E7 Vinyl Dimethicone 1000000 145
vIII E8 Dimethiconot 80000 10000
IX E9 Dimethiconol 60000 11000
X E10 Vinyl Dimethicone 60000 6000
The yams properties of Treated Jute by organopolysiloxane Emulsion (E2) of Example n above, which was used to treat jute and the yarn properties achieved were ascertained which were compared with the fibres treated with conventional JBO as detailed hereunder in Table 2

able 2 Softener Formulation QTY In Kg Type of jute used
Organopolysiloxane emulsion E II 18 Tossa Grade 4 36% Tossa Grade 5 64%
Anionic surfactant 1
Non-ionic surfactant (Detergent P4D 4
Urea 2 Application
Soda Ash 0.2 20-22%
Water 974.8
1000
Tests Emulsion E Iterated fibre JBO treated fibre
1. Piling Period. Hr 24-32 24-32
2. Grist at 16% M.R. (Ib) 10.15-10.45 10.25 -10.80
3. Quality Ratio (%) 81.34 69.81
4, Strength C. V. (%) 19.8 19.65
5. Oil content (%) 0.1 2.6
The Sacking (Warp) properties of Treated Jute by Organopolysiloxane Emulsion E2 of Example II were also noted and compared with that of JBO based treatment and the results are shown hereunder in Table -3
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Table 3
Softener Formulation

QTY In Kg

Type of Jute used

Organopolysiloxane of Emulsion E II 18 Tossa Grade 4 36%
Tossa Grade 5.64%
Anionic surfactant 1
Non-ionic surfactant (Detergent P40) 4
Urea 2 Application

Soda Ash 0.2 20-22%

Water 974.8
1000
Tests JBO treated fibre


1. Piling Period. Hr 24-32 24-32
2. Breaker Card dropping (%) at 16% M.R. 0.55 0.67
3. Finisher Drg. Silver wt. (Ib) at 18% M.R. 144 144
4. Spg. Breaks / 100 spl./hr 45 70
5. Oil content 0.1 2.6
6. Grist at 16% M.R. (Ib) 10.15-10.45 10.25-10.80
7. Quality Ratio (%) 81.34 69.81
(Air Flow Method)
8. Strength C.V. (%) 17.2 16.5
9. Av. Tensile strength, Kgf 3.8 3.2

Further comparison study of Sacks, treated by Emulsions. (El) to (E10) of Examples I to X having different Organopolysiloxane emulsion were studied and the results compared with the JBO treated Sacks detailed hereunder in Table 4 TABLE 4
Tossa Grade 4 Tossa Grade 5
Application
20-22%
36% 64%
Tvne of Jute used
Organopolysiloxane emulsion 18
Anionic surfactant 1
Non-ionic surfactant 4
Urea 2
Soda Ash 0.2
Water 974.8 1000
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Exa mple Orga nopo lysilo xane Emul sion Piling hr. Breaks Card droppin 9(%) Spg. Breaks/ lOOspl/ hr Grist.Ib Tensile Strength Quality Ratio (%) Stren gth C.V. (%)
I El 24-32 0.67 43 10.25 3.8 82 17
II E2 24-32 0.55 44 10.15 3.8 82 17.2
m E3 24-32 1.5 88 10.5 3.8 75 20
IV E4 24-32 1.1 60 10.8 3.6 73 23
V E5 24-32 0.55 70 10.7 3.5 72 22
VI E6 24-32 1.1 90 10.9 3.7 75 21
vn E7 24-32 0.55 42 10.2 3.8 82 18
vm E8 24-32 0.8 76 10.6 3.7 77 24
IX E9 24-32 0.9 74 10.7 3.6 74 25
X E10 24-32 0.8 87 11 3.6 72 25
The above results under Tables 1 to 4 it dearly reveal that after application of above organopolysiloxane emulsions of the invention in the jute processing without any JBO, a wide improvement in properties was noted vis-a-vis when jute was processed with JBO. It has also been found that the raw jute could be easily processed without any interruption by using all varieties of the organopolysiloxane emulsions (El to E10) of the invention in commercial trials. Out of all trials, performance of the emulsions, like El, E2 and E7 are found very good compared to other organopolysiloxane emulsions. It is observed emulsions like El, E2 and E7 are not only better in low oil contents but also improved in tensile strength and breakage of yam during spinning. These properties of organopolysiloxane emulsions favour dramatically cost-effective production of jute in comparison to traditional JBO . Organopolysiloxane used for the jute processing of the invention are absolutely non-toxic, inert, and highly stable in wide range of temperature and processing cost can be reduced 15-20% due to small requirement (0.1%) of organopolysiloxane for effective lubrication and softening of the fibres.
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WE CLAIM:
1) A stable organopolysiloxane emulsion/bath liquor for the lubrication and softening of
lignocellulosic fibres such as jute and allied fibres having particle size up to 10
micron comprising:
a selective formulation comprising (a) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt. (b) water in an amount of 20 to 75 % by wt. (c) selective non-ionic emulsifier(s) having HLB in the range of 10-19 in amounts of 1 to 15% by wt. and (d) selective anionic emulsifier having HLV in the range of 8 -19 in an amount of 1 to 15 % by. wt..
2) A stable organopolysiloxane emulsion/bath liquor as claimed in claim 1 comprising
wetting agent/s preferably in a ratio of 1 part organopolysiloxane emulsion and 0.2
parts wetting agent/s to 1 part organopolysiloxane emulsion and 0.5 part wetting
agent/s.
3) A stable organopolysiloxane emulsion/bath liquor as claimed in anyone of claims 1
to 2 comprising organic fertilizer preferably with an inorganic control releasing agent
favouring the organopolysiloxane penetration to root portion of raw jute fibre.
4) A stable organopolysiloxane emulsion/bath liquor as claimed in claim 3 wherein said
organic fertilizer comprises an amine based fertilizer preferably selected from urea
and derivatives of urea and in amount of from 0.1% to 2.0% for the root processing
and alkali metal salt in a small amount in the range of 0.01% to 1% selectively
provided as control release agent for the fertilizer.
5) A stable organopolysiloxane emulsion/bath liquor for the lubrication and softening of
jute and alike fibres comprising:
(a) 0.5 % to 10% organopolysiloxane emulsion comprising a selective
formulation comprising (i) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt 00 water in an amount of 20 to 75 % by wt. (iii) selective non-ionic emulsifier(s) having HLB in the range of 10-19 in amounts of 1 to 15% by wt. and (iv) selective anionic emulsifier having HLV in the range of 8 - 19 in an amount of 2 to 15 % by. wt..;
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(b) welting agent/s in a ratio of 1 part organopolysiloxane emulsion and 0.2 parts wetting agent/s to 1 part organopolysiloxane emulsion and 0.5 part wetting agent/s;
(c ) organic fertilizer with an inorganic control releasing agent favouring the organopolysiloxane penetration to root portion of raw jute fibre; and
(d) balance made up with water.
6) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1
to 5 wherein Low molecular organopolysiloxane is preferably selected form alpha
omega hydroxy terminated organopolysiloxane; alpha omega alcoxy terminated
organopolysiloxane; cydo organopolysiloxane or mixture thereof.
7) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1
to 6 wherein in case of branched polysiloxane emulsion incorporating a tri functional
or tetra functional silane or a mixture thereof in amounts from 0.1 to 5% depending
on the degree of branching in siloxane molecule.
8) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1
to 7 wherein the alpha omega functional end blocked linear organopolysiloxane are
preferably those of the general formula I:

wherein R1 hydrogen or a monovalent hydrocarbon group of 1 to 10 carbon atoms or a hydroxyl group or an alcoxy group having lto 8 carbon atom; wherein R, which may differ, is a monovalent hydrocarbon radical; and x is an integer from 1 to 100.
9) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1 to 8 wherein the organocydopolysiloxanes comprises of the following structure:

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Where R is the independently hydrogen or monovalent hydrocarbon groups of 1 to 8 carbon atoms including an alkyl group Preferably selected from odamethylcydotetrasiloxane; decamethyicydopentasiloxane; Dodecamethyl cyclohexasifoxane; 1,2,3,4- tetramethyl-l,2,3,4-tetravinyl cyclotetrasiloxane; 1,2,3,4- tetramethyi~l,2,3,4-tetraphenyl cydotetrasiloxane.
10) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1
to 9 wherein the Organopolysiloxane used comprise branched by way of
incorporation of branching units with said branching units selectively provided to
improve the film forming behavior of organopolysiloxane ,to be trifunctional silane
or tetrafunctjonal silane or a mixture thereof.
11) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1 to
10 wherein the Trifuntional silartes (III) and tetrafuncrjon silanes (IV) have the following structure:
R—Si —(O—R)3 Ill Si — (O—R)4, IV
Where R, which may differ, is a monovalent hydrocarbon radical.
12) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims 1
to 11 wherein the Anionic surfactant is selected from organic sulfonic adds,
preferably selected from alkyl aryl sulfonic add; alkyl aryl polyoxyethylene
sulphonic add; alkyl sulfonic add and alkyl polyoxyethylene sulfonic acid. Structures
of sulfonic adds are as below:
R2C6H4SO3H (V) R2C6H4O(C2H4O)mSO3H (VI)
R2SO3H (VI) R3O(C2H4O)mSO3 H (VIII)
Where R2, which may differ, is a monovalent hydrocarbon radial having at least 6 carbon atoms, most preferable R2 groups, but not limited to the following groups, are hexyl, octyl, decyl, dodecyl, cetyl, stearyl, myristyl, and oleyl. 'm' is an integer from 1 to 25.
13) A stable organopolysiloxane emulsion/bath liquor as daimed in anyone of claims l
to 12 comprising preferably anionic surfactants in amounts of 3 to 10% and having
HLB value between 8-12 selected from octyl benzene sulfonic add; dodecyl benzene
sulfonic add; cetyl benzene sulfonic add; Alpha octyl sulfonic add; Alpha dodecyl
sulfonic add; alpha cetyl sulfonic add; polyoxyethylene octyl benzene sulfonic acid;
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polyoxyethylene dodecyl benzene sulfonic acid; polyoxyethylene cetyl benzene sulfonic acid; polyoxyethylene octyl sulfonic add; polyoxyethylene dodecyl sulfonic acid and polyoxyethylene cetyl sulfonic acid.
14) A stable organopolysiloxane emulsion/bath liquor as claimed in anyone of claims 1 to
13 comprising Non-ionic emulsifiers preferably 3-10% having HLB value in between
10-19 preferably surfactants selected from polyoxyalkylene alkyl ether,
polyoxyalkylene alkylphenyl ethers and polyoxyalkylene sorbitan esters ,
polyethylene glycol octyl ether; Polyethylene glycol lauryl ether; Polyethylene glycol
tridecyl ether; Polyethylene glycol cetyl ether; Polyethylene glycol stearyl ether;
polyethylene glycol nonylphenyl ether; polyethylene glycol dodecylphenyl ether;
polyethylene glycol cetylphenyl ether; polyethylene glycol staerylphenyl ether;
polyethylene glycol sorbitan mono stearate and polyethylene glycol sorbitan mono
oleate.
15) A stable organopolysiloxane emulsion/bath liquor as claimed in anyone of claims 1 to
14 comprising non ionic surfactant(s) have HLB value in-between 12-15 to get an
emulsion of organopolysiloxane having long self life.
16) A process for the manufacture of the stable organopolysiloxane emulsion/bath liquor
having particle size up to 10 micron as claimed in anyone of claims 1 to 15 for the lubrication and softening of lignocellulosic fibres such as jute and allied fibres comprising:
providing said selective formulation comprising (a) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt. (b) water in an amount of 20 to 75 % by wt. (c) selective non-ionic emulsifier(s) having HUB in the range of 10-19 in amounts of 1 to 15% by wt. and (d) selective anionic emulsifier having HLV in the range of 8 - 19 in an amount of 1 tol5 % by. wt.
17) A process for the manufacture of a stable organopolysiloxane emulsion /bath liquor
as claimed in claim 16 comprising:
i) adding said wetting agent/s in a ratio of 1 part organopolysiloxane emulsion and 0.2 parts wetting agent/s to 1 part organopolysiloxane emulsion and 0.5 part wetting agent/s;
ii) adding said organic fertilizer from 0.1% to 2.0% with an inorganic control releasing agent for preferably alkali metal salt in a small amount in the range
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of 0.01% to 1% for improving the organopolysiloxane penetration to root portion of raw jute fibre; and
iii) balance being water.
18) A process for softening and lubrication of lignocellulosic fibres such as jute and
allied fibres comprising:
a) providing a final bath liquor comprising organopolysiloxane emulsion having particle size up to 10 micron in the range of 0.5 % to 10% comprising of (a) organopolysiloxane or mixtures thereof in an amount of 20 to 70 % by wt. (b) water in an amount of 20 to 75 % by wt- (c) selective non-ionic emulsifier(s) having HLB in the range of 10-19 in amounts of 1 to 15% by wt. and (d) selective anionic emulsifier having HLV in the range of 8 - 19 in an amount of 1 to 15 % by. wt. and with addition of (i) wetting agent/s in a ratio of 1part organopolysiloxane emulsion and 0.2 parts wetting agent/s to 1 part organopolysiloxane emulsion and 0.5 part wetting agent/s; and (ii) organic fertilizer from 0.1% to 2.0% with an inorganic control releasing agent for preferably alkali metal salt in a small amount in the range of 0.01% to 1% for improving the organopolysiloxane penetration to root portion of raw jute fibre; and (iii) rest portion made up with water; and
b) subjecting the lignocellulosic fibres, jute /allied fibres, to treatment in said bath liquor for the desired softening of the fibres.
19) A process for softening and lubrication of lignocellulosic fibres as claimed in claim
18 wherein during jute processing, the said bath liquor is preferably applied 20-
25% by weight depending on the grade of the jute.
20) A process for softening and lubrication of lignocellulosic fibres as claimed in anyone
of claims 18 or 19 wherein the particle size of the emulsion is adjusted by
changing organopolysiloxane to emulsifiers ratio and/ or by changing the ratio of
anionic emulsifier and non ionic emulsifier.
21) A process for softening and lubrication of lignocellulosic fibres as claimed in anyone
of claims 18 to 20 wherein Organopolysiloxane emulsion having up to 1 micron is
preferably used to achieve desired softness and lubrication of the jute fibre during
processing.
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22) A process for softening and lubrication of lignocellulosic fibres as claimed in anyone
of claims 18 to 21 wherein said organopolysiloxane emulsion used includes
selective range of said quantity of anionic and non ionic emulsifiers in final bath
liquor which is obtained by first, mixing the anionic to non-ionic in a ratio of 3:0.5
to 4:2 and most preferably 4:0.1 to 4:1.5 with said mixed emulsifiers used in the
bath liquor 0.1% to 5% and most preferably 0.3% to 0.6%.
23) A process for softening and lubrication of lignocellulosic fibres as claimed in anyone
of claims 18 to 22 wherein for required penetration of the organopolysiloxane in
the root area small amount of organic fertilizer in effective amount of 0.1 to 2.0%
preferably 0.1 to 0.8% preferably urea or derivates of user is used in the bath
liquor along with a control release additive alkali metal salt preferably selected
from sodium carbonate, sodium bicarbonate, potassium carbonate, potassium
bicarbonate in the range of 0.01% to 1% preferably 0.01% to 0.05% for slow
release of the fertilizer from the bath liquor.
24) A process for softening and lubrication of lignocelluEosic fibres as claimed in anyone
of daims 18 to 23 wherein for said treatment of the lignocellulosic fibre with said
bath liquor the bath liquor is applied to the fibre preferably by spreading the liquor
over the fibre preferably by spraying through drip feed on the softener machine
and then passing the jute bundles through fluted rollers.
25) A process for softening and lubrication of lignocellulosic fibres as claimed in anyone
of daims 18 to 24 wherein the treated jute is stacked or piled for 24-72 hrs
depending on the grade of jute and humidity and subsequent opening of the piles
for processing through carding, drawing units and subsequently spun into yarns.
26) A stable organopolysiloxane emulsion/bath liquor for the lubrication and softening
of lignocellulosic fibres, its process of manufacture and a process for lubricating
and softening of lignocellulosic fibres such as jute and allied fibres substantially as
herein described and illustrated with reference to the accompanying examples.


Dated the 17th April, 2006

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