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(11) Patent Number: KE 118
(45) Date of grant: 22/11/2000
(12) PATENT
(51) IPC(6): AO1N25/34
(21) Application Number: KE/P/1996/0184
(22) Filling Date: 01/07/1996
(31) Priory Number:
(33) Priory County:
(73) Owner(s):TUCCI ASSOCIATES INC. 347 Sally Road Yardly, PA, 19067, USA
(72) Inventor(s):  TUCCI, Raymond, J. DRY, Nathan, M.
(74) Agent: WARUINGE & WARUNGE Advocates P.O BOX 72384 Nairobi

(54) Title:  SLOW-RELEASE INSECT-REPELLENT FORMULATIONS AND USES
(57) Abstract
Slow-release formulations comprising the insect repellentN, N-diethyl-m-toluamide are disclosed. Also disclosed are fabric substrates which are treated with the formulations of the invention. Methods for preparing the formulations, for treating fabric substrates and for repelling insects using same are disclosed.
 
SLOW-RELEASE INSECT-REPELLENT FORMULATIONS AND USES
Field of the Invention
The present invention relates to slow-release micro-capsular insecticidal formulations comprising the insect repellent N, N’ -diethyl-m-toluamide. The invention also relates to woven, non-woven, and knit substrates that are treated with the formulations of the invention.

Background of the Invention
There is a universal need for outdoor fabrics suitable for apparel use and providing for long-term insect repellency. Although many insect repellents are effective when applied to the skin as a spray or lotion, their effectiveness is known to decline with time. Furthermore, in order for an insect repellent to be effective, the insect repellent must be applied in a concentrated amount to a small area of the face, neck, and hands or on selected areas of a wearer's garment.
The effectiveness of insect repellents has been known to improve when such repellents are directly applied to fabrics, which are suitable for outdoor use, and various techniques have been suggested for providing sustained release of an insect control agent.
For example, in U.S. Patent No. 4,056,610 to Barber, et al, the invention provides for a micro-capsular insecticidal composition comprising a pyrethroid and a biological synergist capable of controlling insects for up to four (4) days.

In U.S. Patent No. 5,198,287 to Samson, the invention provi4eli f9r Ion fabric coated on the inside with a composition which renders it water repellent, flame retardant and insect repellent using permethrin as the insect repellent permethrin is protected against oxygen with a plasticizer. The outside of the tent is coated with a composition which renders it water repellent and flame retardant exclusive of the insect repellent. The insect- repellent composition has an effective life of more than six (6) months.
In U.S. Patent No. 4,765,982 to Ronning, the invention relates to compositions devices and methods for controlling insect activity where in insect control agent is self-adhered to a rough-surfaced fiber and provides extended control of insect activity. The microencapsulated insect control agents’ disclosed in Barber are named as the preferred insecticide for use in Ronnings' invention. Ronning teaches that smooth-surfaced fibers do not act as good sites for adhesion of microencapsulated insect control agents.
 
In U.S. Patent No. 5,003,635 to Peterson, the invention relates to elongated flexible insect-repellent strips secured to or retained in cavities in various articles of apparel to repel insects from the person wearing such apparel.

In U.S. Patent No. 4,833,006 to McKinney, the invention relates to a coated fabric that is flame resistant and water repellent and includes a poly-functional isocyanate as an adhesion promoter and binder to adhere the coating to the substrate in a flake proof manner.

In U.S. Patent No. 5,089,298 to McNally, the invention relates to the impregnation of Battle Dress Uniforms (BDUs) used by the U.S. Military with amylopectin fabric wrinkle inhibitor and permethrin insect/arthropod repellent in combination.
In US Patent No. 3,859,121 to Yeadon et al., the invention relates to textiles impregnated with insect- repellent compositions including piperonyl butoxide and pyrethrin, wetting agent, thickener and an agent for preventing migration of the pyrethrin and piperonyl butoxide repellent into foods stored in contact with the textiles and for otherwise retaining the repellent in the textiles.

This invention provides for fabric substrates treated with formulations which comprise an insect repellent such as for example N,N'-diethyl-m-toluamide (DEET)which is known to effectively control a variety of insects. In addition to being an effective insect repellent, DEET is environmentally safe and leaves noharmful residues. DEBT has been found to be stable at both reduced and elevated temperatures and under storage conditions. DEET is effective on biting flies, chiggers, deerflies, fleas, leeches, mosquitoes, and ticks. Several factors influence the efficacy of DEET as an insect repellent, such as, for example, extreme environmental conditions, the extent of absorption and elimination, the type of repellent formulation, and the avidity of the test species. The efficacy of DEET is reduced by increased perspiration rate and the duration of repellent activity is influenced by wash-off, abrasion from the treated surface and absorption. Water, from either rainfall or perspiration, decreases the efficacy of DEET.
Summary of the Invention
It is a primary object of this invention to provide for a slow-release insect-repellent
formulation process of making same comprising an insect-repellent entrapped
in a    matrix such that the insect repellent is slowly released from the matrix. The insect repellent is comprised in microcapsules with a diameter of from 40 about 0.005 Iran to about 1.800 mm.
 
It is a further object of this invention to provide for slow-release insect-repellent formulations and process of making same suitable for treating woven, non- woven and knit substrates.
It is yet another object of this invention to provide for a process for treating a fabric substrate with the insect-repellent formulations of this invention.
It is yet a further object of this invention to provide for a process for repelling insects with the insect- repellent formulations of this invention.
It is another object of this invention to provide for fabric substrates treated with the formulations of this invention with an insect repellency of up to twelve months and a stability comparable to that of consumer apparel.
It is another object of this invention to provide for garments manufactured with the fabric substrates of this invention.
Other objects will appear hereinafter.
Detailed Description of the Preferred Embodiments
Oleophilic silicone compounds, heavy alcohols (such as for example polyvinyl alcohol, airvol, polyvinyl acetate, liquefied synthetic rubber or acrylic copolymers) and the insect repellent N, N-diethyl-m-toluamide (DEET) can be together formulated and spray-dried to form microcapsules in powder form. The formulation has novel properties in that the microencapsulated DEET can be nine released and the rate of release of the DEET can be controlled by varying the
amounts of heavy alcohol or plasticizers used in the process. The DEET can time- release over a period of time spanning of from about 24 hours to about several- months and is affected by the method of storage of the powder and exposure to light and air. It is believed that the time-release of DEET can be attributed to the entrapment of the DEET in the resulting structure of the capsule-forming compounds and the entrapping effect of the silicone elastomers. The time-release property of the DEET and the overall stability of the powder can be affected by further coating the microcapsule with for example a wax compound (bee wax gelatin or polyethylene glycol and derivatives) for an intermediate coating or with for example a ceramic compound (clay, slip, china or ivory) for a harder coating or a protective layer.
Other novel properties of the microcapsules and the powder include solubility in
water and water-based compounds such as for example lotions, crèmes, latex paints, acrylic-based paints and sealers) as well as its solubility in oil, hydrocarbon solvents and the like. It is to be noted that before formulation, all compounds entering into the formulation including DEET were insoluble in water.
 
The insect-repellent formulations of the invention can be applied to a wide range of
fabric substrates without being limited by the coarseness or smoothness of the fabric substrate. As volatility is one of the functional attributes associated with insect repellency, and a high volatility lowers the long term effectiveness of the insect repellent, this invention provides for an insect-repellent formulation which lowers the volatility of the insect repellent thus prolonging its effectiveness.
Furthermore, the insect-repellent formulations of the invention can be combined with a wide range of fabric treatment formulations. The resulting formulations can be applied to any suitable fabric substrate depending on the intended use of the fabric and the fabric treatment process such as, for example, cottons, knits, polyesters or blends, fiberglass, woven or non-woven and heat-sensitive substrates such as acetates and mode-acrylates and nylon. In order to lower the
insect-repellent volatility and control the loss of insect-repellent activity, the formulations can be applied such that multiple layers of super thin laminates are produced and the insect repellent is thus slowly released at each laminate interface as it ruptures.
The slow-release insect-repellent formulation of the invention can be prepared by first formulating the insect repellent N,N'-diethyl-m-toluamide with an oleophilic chemical such as a silicone compound such as for example elastomeric or monomeric silicone, and then by mechanical/ and or chemical entrapment of the resulting compound in a carbohydrate matrix, such as for example a starch compound including but not limited to corn starch, potato starch, technical starch, rice starch and any of the synthetic starches. Silicone, which is immiscible with, water, is dissolved with the DEBT which is also immiscible with water. The DEET-silicone solution is mixed into a starch solution with the resulting solution being miscible in water. The DEBT molecule is entrapped in the lattice-like structure of the starch molecule which has the effect of lowering the vapor pressure of the insect repellent thus reducing its volatility. The DEBT is slowly released from the lattice- like structure of the starch molecule with the net effect of the formation of a slow-release insect-repellent formulation.
In a preferred embodiment, the slow-release insect-repellent formulation consists of from about 40% to about 75% starch, and of from about 10% to about 35% diethyl-m-toluamide, and of from about 15% to about 25% silicone, preferably about 65% starch, about 15% N,N'- diethyl-m-toluamide and about 20% silicone on a dry weight basis. Following spray drying, the slow-release insect-repellent microcapsules have a particle size of from about 0.005 mm to about 1.800 mm.

The slow-release insect-repellent formulation of the invention is prepared by first
dissolving starch in water at its boiling point. The starch solution is cooled to temperature by further addition of water and the insecticide N, N’-diethyl-m-toluamide and silicone are slurried into the starch solution. Following slurrying, the formulation is spray dried using conventional spray drying equipment such that the slurry produces a fine white powder comprising DEET of from about 8% to about 11% and with a moisture of from about 3% to about 8%, total solids of from about 10% to about 15% and little or no odour.
The resultant slow-release insect-repellent formulations of the invention are a non-
irritant to the skin or mucous membranes and are non-toxic. As the following
embodiments describe, the slow-release insect-repellent formulation of the
invention can be formulated for application on fabric substrate in high yields without affecting the functionality, esthetic appearance, hand or feel of the treated substrate and without leaving any residual odour.
In a preferred embodiment, the slow-release the slow release insect-repellent formulation can be combined with a cationic softener and applied as a finishing rinse to a fabric substrate that has been already dyed. The slow-release insect repellent formulation can be combined into a formulation comprising of from about 2% to about 10% on the weight of the fabric (owf) of the slow-release insect- repellent formulation and of from about 2% to about 6% (owf) cationic softener. This formulation can be exhausted onto the fabric substrate under mildly acidic conditions, for example using acetic acid such that the pH is of from about,5..50 to about 6.60 with the slow-release insect-repellent formulation adhering to the cationic sites in dyeing and the cationic softener adhering to the fabric substrate.
In another preferred embodiment, the slow-release insect-repellent formulation composition can be combined in a formulation comprising of from about90% to about 98% (owf) of a padding formulation and of from about 2% to about 5 10% {owl) of the slow-release insect-repellent formulation.
In another preferred embodiment, the slow-release insect-repellent formulation can be combined in a formulation comprising of from about 90% to about 98% (owf) of a pigment printing paste formulation and of from about 2% to about 10% (owf) of the slow-release insect-repellent formulation. The slow-release insect-repellent formulation cross-links with the pigment binder during pigment dyeing and printing to link on to the cellulose groups of the fabric substrate.
 
In another preferred embodiment, the slow-release insect-repellent formulation can be combined in a formulation comprising of from about 90% to about 98% (owf) of water-repellent formulation and of from about 2% to about 10% (owf) of the slow-release insect-repellent formulation.

In another preferred embodiment, the slow-release insect-repellent formulation can be used in a final rinse formulation. Fabric substrates after dyeing, pigment padding and printing, with the appropriate formulation which comprises the slow-release insect-repellent formulation of the invention, can be given a resin finish for hand, appearance and dimensional stability. In this particular embodiment, the resin finish acts as a super thin laminate and provides the treated fabric with an insect-repellent finish and more particularly when the resin used is urea formaldehyde by the cross-linking of the molecular structure of the cotton fibre to the cellulose fibre during resin curing conditions. The slow-release insect-repellent formulation is trapped during the reaction of the urea- formaldehyde with the cellulose molecule in the cotton fabric. hi a preferred embodiment, substrate fabrics of 100% cotton and a 50/50 polyester/cotton blend can be treated with a resin finish comprising of from about 2% to about 5% (owf) of the slow-release insect-repellent formulation of the invention and of about 95% to about 98% (owl) of a resin finish formulation.

In another preferred embodiment, the slow-release insect-repellent formulation can be used in heat transfer printing using a wide range of substrate fabrics. In a preferred embodiment, of from about 2% to about 10% weight/ weight (w/w) of the slow-release insect-repellent formulation can be combined with of from about 2% to about 5% (w/w) ink dispersion and with from about 85% to about 96% (w/w) extender. The fabric was processed by heat transfer printing, i.e., by vaporization of the dye from the paper to the fabric at the sublimation temperature of the dye.
In another embodiment, the ink dispersion can omitted and 100% (w/w) extender can be used. In both cases, the adhesion of the heat transfer paper to the fabric prevents the insect repellent from volatilizing and escaping resulting in greater durability.
From about 2% to about 10% (w/w) of the slow- release insect-repellent formulation of Example I can be combined with about 100% extender. The fabric was processed by heat transfer printing, i.e., by vaporization of the dye from the paper to the fabric at the sublimation temperature of the dye.
Example I
In this example, an insect-repellent formulation can be prepared by mixing into a 40 starch slurry a mixture of silicone about 4% (w/w) and the insect-repellent N,N'-diethyl-m-toluamide about 8% (w/w) . The starch slurry is formed by dissolving about 8% (w/w) starch into about 80% (w/w) water at its boiling point. The mixture of insect repellent and silicone is added to the starch mixture after cooling the slurry to room temperature.

The resultant slimy is spray dried in a spray-drying chamber at an inlet temperature of about 230°F using art-atomizing force of from about 2400 to about 3200 psig from a cocurrant atomizer. The slurry produces a fine white powder comprising of from about 0.1% to about 25% DEET and with about 5% moisture and about 15% total solids.
Example II
From about 2% to about 10% (owf) of the slow- release insect-repellent formulation of Example I can be combined with about 2% (owf) cationic softener (for example, Alpha Soft GMR from Alpha Chemical) and exhausted on a fabric substrate that has been dyed on a jig, beck or jet at about 120°F, for about fifteen (15) minutes and at a pH of from about 5.50 to about 6.60, adjusted with acetic acid.
Example III
From about 2% to about 10% (owf) of the slow- release insect-repellent formulation of Example I can be combined with a pigment padding formulation of about 0.06% (owl) aqueous ammonia, about 4.78% (owf) padding emulsion (for example, padding emulsion #8908 from BASF), about 2.39% (owf) antimigran (for example, antimigrant #09-99515 from BASF), about 0.48% (owf) assenonium sulphate, water, and a variable weight percent of a pigment dye depending out the shade. The resulting formulation is padded on to the fabric at from about 85% to about 90% wet pick up, dried at about 275°F and cured at about 340P, for about thirty (30) seconds.

Example IV
From about 2% to about 10% (owl) of the slow- release insect-repellent formulation of Example I can be combined with a printing formulation of about 4.7% (owf) of a dispersion of an acrylic components in mineral oil (for example, Allied DP3-5205 from Allied Colloidst Inc.) about 10% (owf) white aqueous-based acrylate copolymer emulsion for example, Allied PB-8A from Allied Colloids, Inc.), about 833% (owf) water, and a variable weight percent of a pigment print dye depending on the shade. The resulting formulation is printed onto the fabric in all colours of the pattern and cured at about 340°F for about sixty (60) seconds.
 
Example V
From about 2% to about 10% (owl) of the stow- release insect-repellent formulation of Example I can be combined with a water repellent formulation of about 3.6% (owl) silicone softener (for example, Alpha Chem) SW-I from Alpha Chem), about 6% (owl) wax emulsion (for example, fluoropolymer wax emulsion PEL-TEK 508, Hydrolabs, Inc.), and about 7.2% (owl) of a glyoxal reactant (for example, REACTEX #7222 from Ivax Industries, Inc.). The resulting formulation is padded onto the fabric at about 85% to about 90% (owt) wet-pickup, dried at to about 275°F and cured at about 340°F for about twenty (20) seconds.
example VI
From about 2% to about 10% (owl) of the slow- release insect-repellent formulation of Example I can be combined with a resin finishing composition suitable for treating 100% cotton and comprising about 3.6% (owf) cationic , softener, about 1.2% (owf) silicone softener, and about 9.6% (owl) glyoxal reactant.
From about 2% to about 10% (owl) of the slow- release insect-repellent formulation of Example I can also be combined with a resin finishing composition suitable for treating 50/50 polyester/cotton and comprising about 3.6% cationic softener, about 1.2% (owf) silicone softener, and about 2.4% (owl) glyoxal reactant.
The resin finishing formulation can be applied to a fabric substrate that has been dyed, pigment padded, and/or printed as in the above Examples. The resin finish acts as a super thin laminate and provides an additional insect-repellent coating, With both formulas and fabrics, the chemical mixture is padded on at from about 85% to about 90% wet pickup, dried at about 275°F and cured at about 344109rar twenty (20) seconds.
Example VII
From about 2% to about 10% (w/w) of the slow- release insect-repelloar formulation of Example I can be combined with about 2% ink &spool& and abeet 85% ex- tender. The fabric was processed by heat transfer printing, i.e., by vaporization of the dye from the paper to the fabric at the sublimation temperature of the dye.
Example VIII
From about 2% to about 10% (w/w) of the slow- release insect-repellent formulation of Example I can be combined with about 100% extender. The fabric was processed by heat transfer printing, i.e., by vaporization of the dye from the paper to the fabric at the sublimation temperature of the dye.
Field Testing
The slow-release insect-repellent formulations of the invention were found to afford the wearer complete protection under all types of weather and infestation conditions. Furthermore, the insect-repellency effectiveness of the fabric substrate treatment was found to span up to a period of about several hours to about twelve (12) months.
To test the stability of the fabric treatment, garment were produced from treated fabric. Fabric substrates which were laundered from ten (10) to fifty (50) launderings continue to exhibit insect-repellent properties. It is to be noted that the industry standard number of washings for apparel is three (3), five (5), or ten (10) for consumer apparel and fifty (50) washings for military or certain specialty requirements such as, for example, flame retardancy.
To test the effectiveness of the treatment, laboratory size knit and woven fabric samples were processed using the formulations described above. A first batch of the samples were tested for direct insect repellency using fireants and fruit flies as test insects. For several hours the fireants and fruit flies were directly repelled by the fabric samples. A second batch of the fabric samples were tested by wearers who wore shirts made from the fabric sample. Mosquitoes and blackflies were repelled for at least eleven (11) hours during a fishing trip.
A production trial was initiated on four (4) fabric substrates, knit and wove cotton, poly/cotton and poly/nylon. The fabrics were dyed with the slow-release insect-repellent formulation applied during dyeing or resin finishing as one type of group of fabrics. Another group of knitted and woven fabrics were pad dyed, printed and resin finished with the slow-release insect-repellent formulation applied the dyeing, printing and resin finishing steps.
Garments such as shirts, hats, and the like were produced from the treated fabric substrates. The garments were tested under conditions encountered during outdoor activities. The garments were found to repel insects under outdoor conditions during activities such as hiking, bunting, and fishing in coastal, piedmont and mountain conditions during day and night wear. The treated garments were compared to untreated counterparts under the same conditions. In one particular field trial, garments were tested on mosquitoes. The mosquitoes would land on exposed skin and promptly bite. By contrast, when the mosquitoes landed on the treated fabric at any location on the garment, they would only remain for about four (4) to about six (6) seconds before taking off.
This invention and many of its attendant advantages will be understood from the foregoing description, and it will be apparent that various modifications and changes can be made without departing from the spirit and scope of the invention or sacrificing all of its material advantages, the process hereinbefore described being merely preferred embodiments.
For example, the slow-release insect-repellent formulation of the invention can incorporate different insect control agents such as, for example, permethrin and more generally alkylamides and alkyl-neodecaniides. Additionally, the slow-release insect-repellent formulation can be applied on a wide range of fabric substrates including but not limited to textile blends, woven and non- woven, knits, fibers, leather and synthetic adaptations of leather, flocked fabrics, wood and wood derivatives, plastic and laminates, cable, sheeting, film fiberglass and Plexiglas. The slow-release insect-repellent formulation can be also be comprised in moth proofing formulation, packaging material, and paint formulations. Furthermore, with hard covered capsules, a longer-term repellency can obtained when such capsules are used in the manufacture of commercial finishes such as caulking formulations, paint sealers, wall and floor coverings and the like. Additionally, the formulations of the invention can have a wide applicability in situations requiring a lower concentration of DEET. As an example, the slow-release insect-repellent formulation can be incorporated with a scent or a fragrance or pheromones or with any other formulations that could be conducive to applications in sporting, farming, or hunting situations. Conversely, higher concentrations of up to from about 20% to about 25% solids of the repellent can be used in caulking compounds.
The present invention may be embodied in other specific forms without departing from its spirit or essential attributes. Accordingly, reference should be made to the appended claims, rather than the foregoing specification, as indicating the scope of the invention.
 
CLAIMS
1. An insect-repellent formulation suitable for treating a fabric substrate, including woven, non-woven and knit substrates, said formulation comprising of an insect repellent, reactive silicone and starch, wherein said  constituents of said formulation combine to entrap said insect-repellent such that said insect repellent is released over time.
2. The formulation of claim 1, wherein said constituents of said formulation are present in amounts ranging from 10% to 35% by weight insect-repellent, 10    15% to 25% by weight reactive silicone and 40% to 75% by weight starch.
3. The formulation of claim 1, wherein said starch of said insect-repellent formulation is modified starch.
4. The formulation of claim 1, wherein said amine insect-repellent of said insect repellent formulation is N, N’-diethyl-m-toluidine.
5. The formulation of claim 1, further comprising a finishing agent, wherein said finishing agent comprises a finishing resin, a cationic softener and a wax emulsion.
6. The formulation of claim 5, wherein said finishing resin is selected from the group consisting of glyoxal resins, urea-formaldehyde resins, acrylic resins, polyvinyl acetates, polyvinyl alcohols, melamine, and fluorocarbon resins.
7. Use of the formulation according to claims 1 to 6 characterized by it serves to form an insect-repellent printing paste when 90% to 98% on weight of fabric substrate (owf) of pigment printing paste is combined with 2% to 10% (owl) of said formulation and applied to said substrate.

8. Use of the formulation according to claims 1 to 6 characterized by it serves to form an insect-repellent, water repellent agent when 2% to 10% (owl) of said formulation is combined with 90% to 98% (owl) of a water-repellent formulation and applied to said substrate.

9. Use of the formulation according to claims 1 to 6 characterized by it serves to form an insect-repellent padding when 2% to 10% (owl) of said formulation is combined with 90% to 98% ( owl) padding formulation and applied to said substrate.

10.Use of the formulation according to claims 1 to 6 characterized by it serves
to form an insect-repellent resin finish when 2% to 5% (owf) of said formulation is combined with 95% to 98% (owf) of a resin finish formulation and applied to said substrate, wherein said substrate comprises 100% cotton or a 50/50 polyester/cotton blend.
11.Use of the formulation according to claims I to 6 characterized by it serves to form an insect-repellent formulation in heat transfer printing when 2% to 10% weight/weight (w/w) of said formulation is combined with 0% to 5%  (w/w) ink dispersion and 88% to 96% (w/w) extender and applied to said substrate.
12. Use of the formulation according to claims I to 6 characterized by it serves to form an insect-repellent article of manufacture when said formulation is prepared as an aqueous dispersion and applied to said substrate at from 2% to 30% (owf).
13.Use of the formulation according to claims I to 6, further characterized by it
serves to form an insect-repellent article of manufacture when said %mutation is prepared as an aqueous dispersion and said aqueous dispersion is dried into a powder.
14.Use of the formulation according to claim 13, further characterized by adding an effective amount of said powder to a dye bath and dyeing said substrate 15.17se of the formulation according to claim 13 further characterized by adding an effective amount of said powder to a print paste and printing with said print paste on said fabric substrate.

16. Use of the formulation according to claim 13 further characterized by adding an effective amount of said powder to a finishing solution comprising a finishing agent and applying the finishing solution to said fabric substrate.
17. A process for the manufacture of an insect repellent fabric substrate comprising the steps of forming an aqueous dispersion of the constituents of the formulation according to claims I to 6 and applying from 2% to 30% of said aqueous 4ispersion to said fabric substrate.

18. A process as in claim 17, further comprising the step of drying said aqueous dispersion.
19. A process as in claim 18, wherein said aqueous dispersion is dried prior to applying it to said fabric substrate.
20. A process as in claim 17, wherein said aqueous dispersion is dried into a powder.
21. A process as in claim 20, wherein said powder is formed by spray drying
said aqueous dispersion.
22. A process as in claim 20, further comprising the steps of adding an effective amount of said powder to a dye bath and dying said fabric substrate.

23. A process as in claim 20, further comprising the steps of adding an effective amount of said powder to a print paste to form a print paste mixture and printing on said fabric substrate using said mixture.
24. A process as in claim 20, further comprising the steps of adding an effective
amount of said powder to a finishing solution comprising a finishing agent and applying said finishing solution to said fabric substrate.

 

 

 

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