Title of Invention

ACRYLIC PERFUMED FIBER AND A METHOD OF MAKING THEREOF

Abstract An acrylic fiber having perfume and a method of making thereof is disclosed. Micro-reservoirs are formed in the fibers in which the perfume constituents are embedded.
Full Text FORM - 2
THE PATENTS ACT, 1970
(39 OF 1970)
AND
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10; rule 13)
ACRYLIC PERFUMED FIBER AND A METHOD OF MAKING
THEREOF


ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD.
an Indian Company of Aditya Birla Center, 2nd floor, C Wing, S. K. Ahire Marg, Mumbai 400 025,
Maharashtra, India
THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED.


Field of the invention
The present invention relates to textile fibers.
Background of the invention
The term "fiber" or "textile fiber" means a substance which is capable of being spun into a yarn or made into a fabric by bonding or by interlacing in a variety of methods including weaving, knitting, braiding, felting, twisting, or webbing, and which is the basic structural element of textile products.
Fibers are classified on the basis of their length such as short fibers or staple fiber and long fibers or filament fiber. The fibers can also be classified on the basis of their origin such as natural fibers and man-made fibers. The term natural fibers means any fiber that exists as such in the natural state e.g. vegetable fibers or wood fibers. The other type of fibers is obtained from chemical substances. These are called man made fibers. They are rayon, polyester, nylon, acrylic (cashmilon) and the like.
For centuries, mankind has relied upon various plants and animals to provide raw materials for fabrics and clothing. In recent times, the industrialization and scientific advancement has provided several improved materials having far superior properties, particularly suitable for clothing.
Acrylic fibers are synthetic fibers containing at least 85% of acrylonitrile monomer. The acrylic fibers are prepared from a polymer Polyacrylonitrile which is obtained by free radical polymerisation with an average molecular weight of-100,000. Typical properties of acrylic fibers include, resistance
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to moths, oils, and chemicals. Furthermore, they are also resistant to
deterioration from sunlight exposure.
The process steps involved in the preparation of Acrylic fibers are as
follows:
The Polyacrylonitrile is dissolved in solvents like N,N-dirnethylformamide
or aqueous sodium thiocyanate. Then it is metered through a multi-hole
spinnerette and the resultant filaments are coagulated in an aqueous solution
of the same solvent. The resultant filaments are washed, stretched, dried and
crimped to obtain final acrylic fibers. Acrylic fibers are typically produced
in a range of deniers from 1 to 15.
Acrylic is lightweight, soft, and warm, with a wool-like feel. It dyes very
well and has excellent colorfastness. It is resilient, retains its shape, and
resists shrinkage and wrinkles. Acrylic fibers are commonly used in
sweaters, hand-knitting yarns, rugs, awnings, boat covers, and beanies; the
fiber is also used as a precursor for carbon fiber.
From the spun or filament yarn, fabric is formed by knitting or weaving operations. Knitted fabrics can be made by using hooked needles to interlock one or more sets of yarns through a set of loops. The loops may be either loosely or closely constructed, depending on the purpose of the fabric. Knitted fabrics can be used for hosiery, underwear, sweaters, slacks, suits, coats, rugs and other home furnishings. Weaving is performed using either weft or warp processes.
Some typical preparations that are involved in the weaving operations are warping, slashing or sizing. Sizing agents are added to the yarn by solution or pad/dry techniques. Differences in raw materials, processing chemicals,
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fiber diameter, post treatments and blend ratios can be manipulated to produce a fiber having customized properties suitable for desired application. It is often desired that the acrylic fabrics possess typical properties such as thermal stability, ability to retain perfumes, antibacterial properties and the like. These properties are essential in several industrial as well as household applications. There has been a considerable interest in developing such materials. In order to impart various desirable properties to the fabric as mentioned above to the fabric, several constituents with various properties are added. Such constituents include antimicrobial agents, deodorizing agents, antistatic agents, perfumes. Besides such specific constituents, generic constituents for improving overall quality of the fabric, such as sizing agents, antimicrobial constituents for increasing yarn softness and pliability are also added.
Prior Art:
US 7012053 discloses a process for producing treated fabric which involves application of composition, comprising fabric care additive, perfume, color restoring agent and antimicrobial agent by means of spraying, soaking or dipping.
US 5656333 discloses a method of producing an absorbent nonwoven article which comprises coating of fibers with binder containing colorants, softeners, fragrances, fillers and bactericidal agents.
US 5690922 discloses process for preparation of deodorizable fibers which involves incorporation of powder composition containing deodorizable
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material such as photocatalyst, phosphate of a tetravalent metal and hydroxide of a divalent metal into the polymer.
US 6335075 discloses a multilayer carpet having a deodorizing function. Deodorant is applied by spraying or foaming on one of the layers while it is kneaded on the other layers.
Earlier known processes of incorporating such additives, as reported in the above mentioned patents/applications, mainly involved conventional methods like spraying, encapsulating, solvent spinning, chemical treatment, surface coating and embedding. However, these methods suffer from several disadvantages which include non-uniform and improper adhesion of additives onto the fiber material and gradual washing out of the additives over a period of time and which further affects the feel and texture of the fabric.
There is thus felt a need for a process of incorporating additives to fabric which overcomes these shortcomings.
Objects of the Invention
It is an object of this invention to provide perfumed acrylic fibers, wherein at least one perfume constituent is incorporated in the body of the fiber.
Another object of this invention is to provide a process of incorporating perfume constituents into acrylic fibers which ensures uniform distribution of the perfume constituent throughout the fiber length.
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Yet another object of this invention is to provide perfumed acrylic fibers wherein the perfume constituents are retained in the acrylic product over a prolonged period of time.
Yet another object of this invention is to provide a process of incorporating perfume constituents to acrylic fibers which does not alter the feel and texture of the fabric.
Still another object of this invention is to provide a process of incorporating perfume constituents to acrylic fibers such that inherent properties of the acrylic rayon fibers such as fiber strength, linear density, tenacity, heat resistance, dyeability and drying properties are not altered.
Definitions:
As used in the present specification, the following words and phrases are
generally intended to have the meanings as set forth below, except to the extent that the context in which they are used indicates otherwise.
"Non-aqueous phase" means a melted mixture in liquid state which is water insoluble.
"Aqueous phase" means substance dissolved in water.
" Acrylic Polymer" means acrylic and modacrylic polymers, containing atleast 35% acrylonitrile as a monomer. The other monomers can be methylacrylate, ethyl vinyl ether, vinyl bromide, vinyl chloride, vinyledene
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chloride, vinyl acetate, vinyl sulfonic acid, itaconic acid, and/or methylmethacrylate and sulfonated monomers such as sodium styrene sulfonate, sodium methallyl sulfonate, sodium sulfophenyl methallyl ether
"Acrylic Polymer dope" means an intermediate material in the manufacture of acrylic products that is used for preparation of fibers.
"Preform mass" means an intermediate material suitable for making fibers. "Perfume constituent for example citrus musk" means a group of compounds which when mixed together provides the scent referred to commercially as citrus musk.
Summary of the Invention
In accordance with this invention there is provided a perfume acrylic formulation meant for manufacture of acrylic products comprising:
■ at least one non-aqueous solvent in the range of about 0.01 to 7% of the mass of the formulation,
■ at least one water insoluble perfume constituent soluble in solvent, in the range of about 0.001 to 3.5% of the mass of the formulation ,
■ at least one water soluble nonionic surfactant having HLB value in the range of 9 to 40, in the range of 0.001 to 3% of the mass of the formulation,
■ a solvent for acrylic polymer in the range of 20 to 60% of the mass of the formulation,
■ acrylic polymer in the range of about 1 to 15% of the mass of the formulation, and
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■ water in the range of about 5% to 60 % with respect to the mass of the formulation.
Typically, the perfume constituent is at least one selected from a group consisting of citrus musk, floral woody, citrus musk woody, fresh bouquet, musk ,floral musk, cedarwood oil, sandalwood oil, lemon oil, orange oil, rose oil, jasmine oil and lavender oil.
Typically, the solvent is at least one solvent selected from a group of solvents consisting of C10-C44 alkanes (paraffmic hydrocarbons), polyethylene, polypropylene, polypropylene glycol, polytetramethylene glycol, polypropylene malonate, polyneopentyl glycol sebacate, polypentane glutarate, polyvinyl myristate, polyvinyl stearate, polyvinyl laurate, polyhexadecyl methacrylate, polyoctadecyl methacrylate, polyethylene oxides, polyethylene glycols, Arachidyl alcohol, behenyl alcohol, Selachyl alcohol, chimimyl alcohol, polyesters, di-iso decyl phthalate, benzyl alcohol, C4 -C30 aliphatic alcohols ,C4 -C30 saturated hydrocarbons, C4 -C30 monounsaturated hydrocarbons, natural oils, mineral oil paraffins and diethylphthalate.
Typically, the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of phenoxy ethoxylated non-ionic surfactants, ethoxylated alkyl alcohol, Polyethylene-block-Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol
Typically, the phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(8) isooctylphenyl
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ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9)
nonylphenyl ether, Polyoxyethylene(lO) isooctylphenyl ether,
Polyoxyethylene( 12) nonylphenyl ether, Polyoxyethylene( 12)
isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(l00) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole ethoxylate), Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7 (Alkyl polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol ethoxylate glycol ether).
In accordance with one preferred embodiment of the invention, the HLB value of the surfactant is between 16 and 40.
In accordance with one aspect of the invention, the perfume constituent, the solvent and the surfactant are processed to form micro- reservoirs which are embedded into the body of the formulation.
Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm.
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The invention also extends to a perfume acrylic fiber, yarn and fabric manufactured from a formulation in accordance with this invention.
There is also provided a process for preparation of a perfumed acrylic formulation meant for manufacture of acrylic products comprising the following steps:
In accordance with this invention a process of preparation of a perfumed acrylic formulation meant for manufacture of acrylic products comprising the following steps :
• admixing a water-insoluble perfume constituent with a non-aqueous solvent, to form a non-aqueous phase ;
• heating the non-aqueous phase to a temperature in the range of 25°C to 95°C;
• dissolving and stirring a surfactant, optionally with a co-surfactant, a solvent for acrylic polymer in water to obtain an aqueous phase;
• heating the aqueous phase;
• mixing the aqueous phase with the non-aqueous phase in liquid state to form an admixture, and homogenizing to obtain a micro-emulsion;
• mixing the micro-emulsion with an acrylic polymer solution in a
solvent and water and further homogenizing and dispersing the
micro-emulsion to obtain a polymer dope wherein the perfume
constituent is embedded in evenly dispersed micro-reservoirs.
Typically, the pH of the aqueous phase is in the range of 7 to 13.
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Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion.
Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion.
Typically, the proportion of perfume constituent in the acrylic product is in the range of O.OOlto 20% with respect to the mass of the acrylic product.
Typically, the solvent for polyacrylonitrile is at least one selected from a group consisting of sodium thiocyanate , dimethyl formamide, dimethyl acetamide, dimethyl sulfoxide, ethylene carbonate, aqueous zinc chloride and aqueous nitric acid. The polymer percentages in the acrylic dope will vary depending on the solvent. For dimethyl formamide, acrylic polymer concentration soluble in polymer dope is as high as 28-32%; for dimethyl acetamide, it is as high as 22-27%; for dimethyl sulfoxide, it is as high as 20-25%; for ethylene carbonate, it is as high as 15-18%, for aqueous nitric acid, it is as high as 8-12% and for zinc chloride, it is as high as 8-12%. For Sodium thiocyanate as a solvent, acrylic polymer concentration is as high as 10-15%.
Brief Description of the accompanying Drawings:
The invention will be described in detail with reference to the accompanying
drawings.
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In the accompanying drawing, Figure 1 illustrates the block diagram showing the method steps involved in the process in accordance with this invention.
Figure 2 illustrates the cross-sectional view of perfumed acrylic fibers prepared in accordance with this invention which shows uniform distribution of microreservoirs of perfume constituent entrapped across the length of the fibers.
Detailed Description:
Acrylic fibers were the first viable manufactured fibers. The reason behind
the most widespread use of these fibers lies in their versatility. Furthermore,
these fibers also have peculiar ability to blend easily with many fibers which
makes them the fibers of choice.
Though Rayon fibers and fabrics made from them have many desirable
properties, oftentimes, consumers expect performance characteristics beyond
those for which rayon fibers were designed. In order to meet with these
increasing expectations, various perfume constituents are incorporated in the
acrylic fibers. There has been a considerable interest in developing such
materials.
There is enormous demand for acrylic fibers with intrinsic perfume.
In accordance with this invention there is provided a perfumed acrylic
formulation meant for manufacture of acrylic products comprising:
■ at least one non-aqueous solvent in the range of about 0.01 to 7% of the mass of the formulation,
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■ at least one water insoluble perfume constituent soluble said solvent, in the range of about 0.001 to 3.5% of the mass of the formulation,
■ at least one water soluble nonionic surfactant having HLB value in the range of 9 to 40, in the range of 0.001 to 3% of the mass of the formulation,
■ a solvent for polyacrylonitrile in the range of 20 to 60% of the mass of the formulation,
■ acrylic polymer in the range of about 1 to 15% of the mass of the formulation, and
■ water in the range of about 5% to 60 % with respect to the mass of the formulation.
In accordance with the invention, various perfume constituents from different sources are used. The typical perfume comprises a plurality of individual perfume active compounds, although it can consist essentially of a single perfume ingredient. It is well within the scope of the perfumer of ordinary skill in the art changing ingredients in the perfume component and/or modifying the relative levels of perfume ingredients. In case of synthetic perfume constituents, a perfume constituent is a composition of one or more synthetic compounds. Various types of chemical compounds are commonly known for perfumery uses including: phenolic compounds; essential oils; aldehydes; ketones; polycyclic compounds; esters; and alcohols. Many perfume ingredients contain a combination of functional groups and can be categorized under two or more of the above classes.
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Various plant derived perfume constituents generally include variety of phyto-chemicals along with the principle active phyto-constituent.
From the standpoint of the perfumer, it is convenient to consider the perfume ingredients in terms of the type of aroma it imparts rather than the particular chemical class or classes it may fall within. The perfume components herein can be formulated to provide a variety of odor categories: a non-exclusive list includes woody, sweet, citrus, floral, fruity, animal, spice, green, musk, balsamic, chemical, and mint. A variety of exemplary perfume ingredients are described below for several of the commonly used odor categories, long with their representative (but not necessarily exclusive) chemical categories.
Woody perfume ingredients include cedarwood oil (essential oil), guaicwood oil (essential oil), gamma ionone (ketone), sandalwood oil (essential oil), and methyl cedrylone (ketone). Sweet perfume ingredients include coumarin (ketone), vanillin (4 hydroxy-3methoxy benzaldehyde) (aldehyde), ethyl maltol (Alcohol), phenyl acetaldehyde (aldehyde), heliotropin (aldehyde), acetophenone (ketone), and dihydrocoumarin (ketone).
Citrus perfume ingredients include orange oil (essential oil), lemon oil (essential oil), citral (aldehyde), beta methyl naphthyl ketone (ketone), terpinyl acetate (ester), nonyl aldehyde (aldehyde), terpineol (alcohol), and dihydromyrcenol (alcohol).
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Floral perfume ingredients include a variety of floral subcategories, such as rose, lavender, jasmin, and muguet. Rose perfume ingredients include geranyl acetate (ester), geraniol (alcohol), citronelyl acetate (ester), phenyl ethyl alcohol (alcohol), alpha damascone (ketone), beta damascone (ketone), geranium oil (essential oil), and natural rose oil (essential oil). Lavender perfume ingredients include dihydro terpinyl acetate (ester), ethyl hexyl ketone (ketone), lavandin (essential oil), lavender (essential oil), terra hydro linalool (alcohol), linalool (alcohol), and linalyl acetate (ester). Jasmin perfume ingredients include benzyl acetate (ester), butyl cinnamic aldehyde (aldehyde), methyl benzoate (ester), natural jasmin oil (essential oil), methyl dihydro jasmonate (ester). Muguet perfume ingredients include cycalmen aldehyde (aldehyde), benzyl salycilate (ester), hydroxycitronellol (alcohol), citronellyl oxyacetaldehyde (aldehyde), and hydroxy aldehyde (aldehyde).
Fruity perfume ingredients include ethyI-2-methyI butyrate (ester), allyl cyclohexane propionate (ester), amyl acetate (ester), ethyl acetate (ester), gamma decalactone (ketone), octaiactone (ketone), undecalactone (aldehyde), ethyl aceto acetate (ester), benzaldehyde (aldehyde).
Animal perfume ingredients include methyl phenyl acetate (ester), indol (2,3, benzpyrrole) (phenolic), creosol (phenolic), iso butyl quinolin (phenolic), and androstenol (phenolic).
Spice perfume ingredients include anisic aldehyde (aldehyde), anise (essential oil), clove oil (essential oil), eugenol (phenolic), iso eugenol (phenolic), thymol (phenolic), anethol (phenolic), cinnamic alcohol (alcohol), and cinnamic aldehyde (aldehyde).
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Green perfume ingredients include beta gamma hexenol (alcohol), brom styrol (alcohol), dimethyl benzyl carbinol (alcohol), methyl heptine cart onate (ester), cis-3-hexenyl acetate (ester), and galbanum oil (essential oil).
Musk perfume ingredients often also function as fixatives. Examples of musk include glaxolide (phenol), cyclopentadecanolide (phenol), musk ketone (ketone), ambrettolide (phenol), tonalid (phenol), and ethylene brassylate (ester).
Balsamic perfume ingredients include fir balsam (essential oil, peru balsam (essential oil), and benzoin resinoid (essential oil).
Mint perfume ingredients include laevo carvone (ketone), menthol (alcohol), methyl salicylate (ester), peppermint oil (essential oil), spearmint oil (essential oil), eucalyptus (essential oil), anisyl acetate (ester), methyl chavicol (alcohol).
Chemical perfume ingredients include benzyl alcohol (alcohol), diproplene glycol (alcohol), ethanol (alcohol), and benzyl benzoate (ester) , Andrane, Cedramber, Decyl methyl ether, Galaxolid, Grisalv, Indolarome-soli, Orange flower ether, Ozofleu, Phenafleu, Tobacaro, Paracresyl methyl Ether, Karana, Cyclogalbanat, Piconi, Iso-cyclemone, Iso E supe, Celestolide-soli, Fleuramon,, ihydroisojasmon, Isojasmon, Tonali, Methyl Ionone , Dulcinyl-soli, Acetanisol, Vetikon, Undecylenic Aldehyd, lilia, Vanilli, Cinnamic Alcoho, Iso-Eugeno, Tetra-Hydro Geranio, Calone 10 % DE, Dihydro-isojasmon, Galaxolide, Karanal 10% DE, Yara Yara (Nerolin)
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, Decyl methyl ether, Ethyl Methyl Phenyl Glycidate, Para-Cresyl Phenyl acetate, Undecalactone, Clonal IFF
Preferred plant derived perfume compositions are provided herein below :
Rose oil : beta-damascenone, beta-damascone, beta-ionone and rose oxide.
Lavender oil : linalool and linalyl acetate.
Orange oil : d-limonene.
Jasmine oil : benzyl acetate, linalool, benzyl alcohol, indole, benzyl
benzoate, cis-jasmone, geraniol and methyl anthranilate.
Sandalwood oil : santalols, santene, nor-tricycloekasantalene and a- and ,B-
santalenes, santenol and teresantalol.
Cedarwood oil : p-methyl-8-3- tetrahydroacetophenone, p-methyl
acetophenone, cis- and trans- atlantones, a- and p-himalchenes, ar-
dihydroturmerone and himachalol.
The perfume constituent impart peculiar pleasant aroma or fragrance to the fibers and ultimately to the fabric or garments made from these fibers.
In accordance with this invention, a non-aqueous solvent is used which is typically selected from a group of solvents consisting of C10-C44 alkanes (paraffinic hydrocarbons), polyethylene, polypropylene, polypropylene glycol, polytetramethylene glycol, polypropylene malonate, polyneopentyl glycol sebacate, polypentane glutarate, polyvinyl myristate, polyvinyl stearate, polyvinyl laurate, polyhexadecyl methacrylate, polyoctadecyl methacrylate, polyethylene oxides, polyethylene glycols, Arachidyl alcohol, behenyl alcohol, Selachyl alcohol, chimimyl alcohol, polyesters, di-iso decyl phthalate, diethyl phthalate and other alkyl phthalates, benzyl alcohol, C4 -
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C30 aliphatic alcohols ,C4 -C30 saturated hydrocarbons, C4 -C30 monounsaturated hydrocarbons, natural oils, mineral oil paraffins and diethylphthalate.
Preferably, paraffin wax either alone or in combination with stearyl alcohol is used as the non-aqueous solvent.
In accordance with this invention a water soluble non-ionic surfactant/co-surfactant is used. Typically, the non-ionic surfactant is selected from a group consisting of phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol, Polyethylene-block-Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol. Typically, the alkyl phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(8) isooctylphenyl ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether, Polyoxyethylene(10) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(100) nonylphenyl ether, Polyoxyethylene(150) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha-(nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) ,Surfonic N-95(Poly (oxy-1, 2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) ( nonylphenol 9.5-mole ethoxylate) , Surfonic N-120(nonylphenol 12-mole ethoxylate) , Surfonic N-150 (nonylphenol 15-mole ethoxylate), Surfonic N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol 30-mole ethoxylate) , Surfonic
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N-400 nonylphenol 40-mole ethoxylate, Surfonic LF-7 (Alkyl
polyoxyalkylene ether) , Surfonic LF-17 (ethoxylated and propoxylated
linear primary 12-14 carbon number alcohol), Igepal CO-630 (nonylphenoxy
poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40 (dinonylphenol
ethoxylate glycol ether).
The non-ionic surfactant is selected such that the lipophilic portion of the non-ionic surfactant is compatible with the perfume constituent and the surfactant forms oil in water micro-emulsion. Surfactants with HLB values within the range of 9 to 40 are used. Preferably, non-ionic surfactants with HLB values more than 13 are used.
In accordance with one preferred embodiment of the invention, the HLB value of the surfactant is between 16 and 40.
In accordance with one aspect of the invention, the perfume constituent, the solvent and the surfactant are processed to form micro-reservoirs which are embedded into the body of the formulation. The perfumed micro-reservoirs are eventually dispersed uniformly throughout the body of the fibers. The micro-reservoirs are discrete, nano-sized structures without any definite geometrical shape.
Typically, the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm.
The invention also extends to a perfume acrylic fiber, yarn and fabric manufactured from a formulation in accordance with this invention.
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In accordance with this invention there is also provided a process for preparation of a perfume acrylic formulation meant for manufacture of acrylic products comprising the following steps:
• admixing a water-insoluble perfume constituent with a non-aqueous solvent followed by heating the resulting admixture to a temperature in the range of 25°C to 950C to obtain non-aqueous phase ;
• dissolving and stirring a surfactant, optionally with a co-surfactant, in water to obtain a aqueous phase;
• admixing and homogenizing the non-aqueous phase with the aqueous phase to obtain a micro-emulsion;
• dispersing the micro-emulsion throughout the mass of the acrylic polymer dope to obtain a preform mass wherein the perfume constituent is in the form of evenly dispersed micro-reservoirs.
Typically, the pH of the aqueous phase is in the range of 7 to 13.
Typically, the amount of non-aqueous phase in the micro-emulsion is in the range of 0.1 to 40% of the mass of the micro-emulsion.
Typically, the amount of surfactant in the micro-emulsion is in the range of 0.1 to 20% of the mass of the micro-emulsion.
Typically, the proportion of perfume constituent in the acrylic product is in the range of 0.001 to 20% with respect to the mass of the acrylic product.
Before arriving at the optimum concentration of the surfactant to be used, cloud point of the aqueous phase is determined. Furthermore, alkalinity of
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the aqueous phase matches with that of the acrylic polymer dope thereby avoiding any drastic change in the alkalinity during the emulsification and homogenization step.
Typically, the melted non-aqueous phase containing perfume constituent in a non-aqueous solvent along with aqueous phase containing surfactants is emulsified using high speed mixers such as Ultraturrex or a mechanical emulsifier; a colloid mill; a high pressure homogenizer and an ultrasonic emulsifier to form a micro-emulsion. The micro-emulsion may contain further additional perfume constituents, if desired.
The active ingredients are released from the micro-reservoir into the acrylic matrix. The structure of micro-reservoir, acrylic and surrounding conditions determine the release rate of the perfume constituent. The molecules of the volatile perfume constituents migrate from micro-reservoirs to the surrounding primarily by diffusion. The perfume constituent is released from the matrix in a controlled release manner.
Preform mass is spun to fiber in a bath containing 12.5% of Sodium thiocyanate solution. The temperature of the bath is maintained at -2.5°C. Thereafter, the fiber is cold stretched, gel treated at pH 2.8 at 45°C, then hot stretch at 90°C.
The void in the fibers is removed by treating the fiber at 125°C. Fiber is then relaxed and annealed at 120°C and then taken up for post-treatment.
The acrylic fibers can be further subjected to post treatment to make fabric which typically involves:
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o Converting to Yarn in blend or pure
o Converting to Warp Beam
o Sizing
o Fabric Manufacturing- Weaving /Knitting
o Dyeing
o Finishing
Alternatively, the filaments so obtained are further blended using standard equipment. The blended fibers are laid in to a web using standard equipment followed by Consolidation of the web to obtain Non-woven Acrylic Fabric.
The acrylic product made from the formulation in accordance with this invention contains uniformly dispersed micro-reservoirs throughout the mass which is shown in Fig. 2.
A typical perfumed acrylic fiber as obtained by the process of this invention contains the releasable perfume constituent entrapped in the form of pockets. Said pockets are uniformly distributed throughout the length of the fiber. Upon microscopic examination, perfume constituent enriched acrylic fiber shows uniform distribution of pockets along the length of the acrylic fiber as shown in Fig. 2.
The resultant perfumed acrylic fabric is tested. Linear Density (Denier) of the acrylic Fibers is determined by using standard ASTM Test Method (D 1577). The denier of the standard acrylic fiber (acrylic fiber without any perfume constituents) and perfume enriched acrylic fiber remains the same. Thus addition of perfume does not change the linear density of the acrylic fibers.
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Tensile strength and Young's modulus of acrylic fiber sample is tested on an Instron tensile testing machine as per the ASTM C1557-03 procedure at ambient temperature.
Visual appearance of the perfume enriched fiber is evaluated by methods as prescribed in AATCC 124. As far as parameters like % Loss in Dry Tenacity and % loss in dry elongation are concerned, these remain the same in the perfume enriched acrylic fiber and the standard fiber. Incorporation of perfume constituent in accordance with this invention does not affect the visual appearance of the fiber.
Feel of the fiber: The perfume enriched acrylic fiber as prepared in accordance with this invention offers the same feel effect as is observed in case of plain acrylic fiber without any perfume constituent (Also referred as standard).
Another important concern in textile industry is dye-ability of the fabric, which is tested by comparing the dyeability of the perfume constituent enriched fabric and the standard acrylic fabric. Dyeability of the perfume enriched acrylic fibers as prepared in accordance with this invention remains the same as that of the standard acrylic fiber.
Perfume retention test:
Perfumed acrylic fabric before and after washes is tested for aroma or fragrance by using expert human panel. Fragrance of the perfumed acrylic fibers as prepared in accordance with this invention was perceived even after repeatedly washing the fabric and exposing it to sunlight and / or varying
temperatures.
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The invention will now be described with the help of the following non-limiting examples.
Examples Example 1
Example 1A- Preparation of micro emulsion
Myristyl alcohol (200gm) and cetyl alcohol (50 gm) were heated upto 50°C
to obtain a molten mixture. To this 25 gm of citrus musk was added to form
a non-aqueous phase (275gm)
Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) (30 gm ) was
dissolved and stirred in water 550 ml and Sodium thiocyanate (250 gm)
to obtain (830 gm) of aqueous phase.
The aqueous phase (830 gm) was heated to the temperature of the molten
non-aqueous phase (275 gm) and both the phases were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion (1105 gm).
Example 1 B- Preparation of fiber
(1105 gm) of micro-emulsion as prepared in Example 1A was mixed at 50°C
with acrylic Polymer Dope containing 5000gm of acrylic polymer and
16670gm of sodium thiocyanate and 20000 ml of water were added to
obtained preform mass.
Preform mass was spun in a bath containing 12.5% of Sodium thiocyanate
solution. The temperature of the bath was maintained at -2.5°C. Thereafter,
the fiber was cold stretched, gel treated at pH 2.8 at 45°C, then hot stretched
at 90°C.
24

The voids in the fibers were removed by treating the fiber at 125°C. Fiber is then relaxed and annealed at 120°C and then taken up for post-treatments and was spun into fiber.
The acrylic fiber thus obtained contained micro-reservoirs having the entrapped releasable perfume constituents. Although the micro reservoirs did not have any specific shape or size, they were found to be uniformly distributed throughout the body of the fiber.
Example 2
Example 2 A- Preparation of micro emulsion
Stearyl (200gm) and cetyl alcohol (50 gm) were heated upto 50°C to obtain a molten mixture. To this 25 gm of floral woody was added to form a non¬aqueous phase (275gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 38 gm ) was dissolved and stirred in water 550 ml and Sodium thiocyanate (250 gm) to obtain (838 gm) of aqueous phase. The aqueous phase (838 gm) was heated to the temperature of the molten non-aqueous phase (275 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1113 gm).
Example 2 B- Preparation of fiber
(1113 gm) of micro-emulsion as prepared in Example 2A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass and the fiber was obtained by the process as described in example 1.
25

Example 3
Example 3 A- Preparation of micro emulsion
Stearyl alcohol (200gm) and Polyvinyl laurate (50 gm) were heated upto 50 C to obtain a molten mixture. To this 100 gm of woody musk was added to form a non-aqueous phase (350gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 30 gm ) was dissolved and stirred in water 525 ml and Sodium thiocyanate (250 gm) to obtain (805 gm) of aqueous phase. The aqueous phase (805 gm) was heated to the temperature of the molten non-aqueous phase (350 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1155 gm).
Example 3B- Preparation of fiber
(1155 gm) of micro-emulsion as prepared in Example 3 A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass and the fiber was prepared by the process as described in example 1 .
Example 4
Example 4A- Preparation of micro emulsion
Stearyl (200gm) and paraffin wax (50 gm) were heated upto 50°C to obtain a molten mixture. To this 75 gm of fresh bouquet was added to form a non¬aqueous phase (325gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) (40gm ) was dissolved and stirred in water 550 ml and Sodium thiocyanate (250 gm) to obtain (840 gm) of aqueous phase.
26

The aqueous phase (840 gm) was heated to the temperature of the molten non-aqueous phase (325 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1165 gm).
Example 4B- Preparation of fiber
(1165 gm) of micro-emulsion as prepared in Example 4A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass.
Example 5
Example 5 A- Preparation of micro emulsion
Stearyl alcohol (300 gm) and Myristyl alcohol (50 gm) were heated upto 50°C to obtain a molten mixture. To this 100 gm of floral musk was added to form a non-aqueous phase (450gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 60 gm ) was dissolved and stirred in water 640ml and Sodium thiocyanate (250 gm) to obtain (950 gm) of aqueous phase.
The aqueous phase (950 gm) was heated to the temperature of the molten non-aqueous phase (450 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1400gm).
Example 5 B- Preparation of fiber
(1400gm) of micro-emulsion as prepared in Example 5A was mixed at50 C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass.
27

Example 6
Example 6 A- Preparation of micro emulsion
Stearyl alcohol (200gm) and Myristyl alcohol (50 gm) were heated upto
50 C to obtain a molten mixture. To this 80 gm of citrus musk was added
to form a non-aqueous phase (330gm).
Surfonic N-400 nonylphenol 40-moie ethoxylate (surfactant) ( 35 gm) was
dissolved and stirred in water 540 ml and Sodium thiocyanate (250 gm)
to obtain (825 gm) of aqueous phase.
The aqueous phase (825 gm) was heated to the temperature of the molten
non-aqueous phase (330 gm) and both the phases were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion (1155gm).
Example 6 B- Preparation of fiber
(1155 gm) of micro-emulsion as prepared in Example 6A was mixed at50 C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass.
Example 7
Example 7 A- Preparation of micro emulsion
Myristyl alcohol (250gm) was heated upto 50°C to obtain a molten mixture. To this 40 gm of citrus musk woody was added to form a non-aqueous phase (290gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 35 gm ) was dissolved and stirred in water 540 ml and Sodium thiocyanate (250 gm) to obtain (825 gm) of aqueous phase.
28

The aqueous phase (825 gm) was heated to the temperature of the molten non-aqueous phase (290 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1115 gm).
Example 7 B- Preparation of fiber
(1115 gm) of micro-emulsion as prepared in Example 7A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass.
Example 8
Example 8 A- Preparation of micro emulsion
cetyl alcohol (250 gm) were heated upto 50°C to obtain a molten mixture.
To this 25 gm of floral woody was added to form a non-aqueous phase
(275gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 28
gm ) was dissolved and stirred in water 550 ml and Sodium thiocyanate
(250 gm) to obtain (828 gm) of aqueous phase.
The aqueous phase (828 gm) was heated to the temperature of the molten
non-aqueous phase (275 gm) and both the phases were homogenized in a
high speed mixer (Ultraturrex) to obtain a micro-emulsion (1103 gm).
Example 8B- Preparation of fiber
(1103 gm) of micro-emulsion as prepared in Example 8A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass and fiber was obtained by the process as described in example 1.
29

Example 9
Example 9A- Preparation of micro emulsion
Stearyl alcohol (200gm) and cetyl alcohol (50 gm) were heated upto 50°C to obtain a molten mixture. To this 25 gm of fresh bouquet was added to form a non-aqueous phase (275gm) Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 35 gm) was dissolved and stirred in water 553 ml and Sodium thiocyanate (250 gm) to obtain (838 gm) of aqueous phase. The aqueous phase (828 gm) was heated to the temperature of the molten non-aqueous phase (275 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1113 gm).
Example 9 B- Preparation of fiber
(1113 gm) of micro-emulsion as prepared in Example 9A was mixed at50°C with acrylic Polymer Dope containing 5000 gm of acrylic polymer and 16670gm of sodium thiocyanate and 3110ml of water were added to obtained preform mass and fiber was obtained by the process as described in example 1.
Example 10
Example 10A- Preparation of micro emulsion
Stearyl alcohol (200gm) and cetyl alcohol (50 gm) were heated upto 50°C to obtain a molten mixture. To this (25 gm) of lavender oil was added to form a non-aqueous phase (275gm).
Surfonic N-400 nonylphenol 40-mole ethoxylate (surfactant) ( 40 gm ) was dissolved and stirred in water 548 ml and Sodium thiocyanate (250 gm) to obtain (838 gm) of aqueous phase.
30

The aqueous phase (838 gm) was heated to the temperature of the molten non-aqueous phase (275 gm) and both the phases were homogenized in a high speed mixer (Ultraturrex) to obtain a micro-emulsion (1113 gm).
Example 10 B- Preparation of fiber
(1113 gm) of micro-emulsion as prepared in Example 10A was mixed at50°C with acrylic Polymer Dope containing 600 gm of acrylic polymer and 16670gm of sodium thiocyanate and 20000 ml of water were added to obtained preform mass and fiber was obtained by the process as described in example 1.
Testing procedures:
The perfumed acrylic products as prepared in the above examples (1 to 10) were tested by using following test procedures;
1) Linear Density (Denier) of the acrylic fibers was determined by using
standard ASTM Test Method (D 1577).
The denier of the standard acrylic fiber (without any perfume constituents) and anti-microbial acrylic fibers as prepared in accordance with example 1B was found to be uniform(l .5 denier) irrespective of the type and quantity of the perfume constituent.
2) Tensile strength and Young's modulus of acrylic fiber samples were tested on an Instron tensile testing machine as per the ASTM C1557-03 procedure at ambient temperature.
3) Emulsion stability: The stability of micro-emulsions as prepared in the above examples, was evaluated by keeping the same under observation
31

in measuring cylinders for 3 days. During this period no phase separation was observed.
4) Feel of the fabric: The acrylic fabrics as prepared in the above examples and standard fabric (acrylic fabric without perfume constituents), were randomly given to twenty subjects and they were asked to evaluate the texture and feel of the fiber. The test fiber material was interchanged several times amongst the human subjects. Collective results as submitted by the human subjects confirmed that nobody could distinguish between the perfumed acrylic fabrics prepared in accordance with the Examples provided above and the standard fabric.
5) Dyeability: The perfumed acrylic fabrics as prepared in the above examples and the standard fabric as described above were dyed uniformly with reactive dyes. No noticeable difference as to the Dyeability of the two respective acrylic fabrics, with and without perfume constituent was reported.

6) Visual appearance of the perfumed acrylic fiber was evaluated by methods as prescribed in AATCC 124. As far as parameters like % Loss in Dry Tenacity and % loss in dry elongation are concerned, these remained the same( 7) Perfume retention test:
Twenty pieces of standard size 20cmX20cm cut out from the freshly prepared acrylic fiber as prepared in accordance with example 1B. Another set of Twenty pieces of the same size cut out of from the same
32

fiber were subjected to 20 hot water washes with the intermittent drying period of 2 hrs. The drying was carried out in natural sunlight at temperature within the range of 25 to 45°C The specimens so prepared were randomly distributed to human subjects for testing the aroma of the specimen. The specimen was interchanged amongst the subjects. The odor of the two respective acrylic fiber specimens was reported as perceivable and therefore it is concluded that the acrylic fiber specimen retained the perfume additive even after exposure to varying conditions.
While considerable emphasis has been placed herein on the specific steps of the preferred embodiment, it will be appreciated that many alterations can be made and that many modifications can be made in the preferred embodiment without departing from the principles of the invention. These and other changes in the preferred embodiment as well as other embodiments of the invention will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation.
33

We Claim:
1. A perfumed acrylic formulation meant for manufacture of acrylic
products comprising :
■ at least one non-aqueous solvent in the range of about 0.01 to 7% of the mass of the formulation,
■ at least one water insoluble perfume constituent soluble said solvent, in the range of about 0.001 to 3.5% of the mass of the formulation,
■ at least one water soluble nonionic surfactant having HLB value in the range of 9 to 40, in the range of 0.001 to 3% of the mass of the formulation,
■ a solvent for polyacrylonitrile in the range of 20 to 60% of the mass of the formulation,
■ acrylic polymer in the range of about 1 to 15% of the mass of the formulation, and
■ water in the range of about 5% to 60 % with respect to the mass of the formulation.

2. A formulation as claimed in claim 1, wherein the perfume constituent is at least one selected from a group consisting of citrus musk, floral woody, citrus musk woody, fresh bouquet, musk , woody, woody musk, floral musk , lavender oil, jasmine oil, rose oil, cedarwood oil, sandalwood oil, orange oil and lemon oil.
3. A formulation as claimed in claim 1, wherein the solvent is at least one solvent selected from a group of solvents consisting of C10-C44 alkanes
34

(paraffinic hydrocarbons), polyethylene, polypropylene, polypropylene glycol, polytetramethylene glycol, polypropylene malonate, polyneopentyl glycol sebacate, polypentane glutarate, polyvinyl myristate, polyvinyl stearate, polyvinyl laurate, polyhexadecyl methacrylate, polyoctadecyl methacrylate, polyethylene oxides, polyethylene glycols, Arachidyl alcohol, behenyl alcohol, Selachyl alcohol, chimimyl alcohol, polyesters, di-iso decyl phthalate, diethyl phthalate and other alkyl phthalates, benzyl alcohol, C4 -C30 aliphatic alcohols ,C4 -C30 saturated hydrocarbons, C4 -C30 monounsaturated hydrocarbons, natural oils, mineral oil paraffins and diethylphthalate.
4. A formulation as claimed in claim 1, wherein the surfactant is at least one non-ionic surfactant selected from a group of non-ionic surfactants consisting of phenoxy ethoxylated non-ionic surfactants and ethoxylated alkyl alcohol, Polyethylene-block-Poly propylene glycol-block-polyethylene glycol and Ethylenediamine tetrakis(propylene oxide-block-ethylene oxide) tetrol.
5. A formulation as claimed in claim 8, wherein the alkyl phenoxy ethoxylated non-ionic surfactant is at least one selected from a group consisting of Polyoxyethylene(8) isooctylphenyl ether, Nonylphenol polyethylene glycol ether, Polyoxyethylene(9) nonylphenyl ether, PolyoxyethyIene(10) isooctylphenyl ether, Polyoxyethylene(12) nonylphenyl ether, Polyoxyethylene(12) isooctylphenyl ether, Polyoxyethylene(40) nonylphenyl ether, Polyoxyethylene(40) isooctylphenyl ether, Polyoxyethylene(100) nonylphenyl ether, Polyoxyethylene(l50) dinonylphenyl ether, Surfonic N-95(Poly (oxy-1,
35

2-ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) (
nonylphenol 9.5-mole ethoxylate) ,Surfonic N-95(Poly (oxy-1, 2-
ethanediyl), alpha- (nonyl phenyl)-omega-hydroxyl-glycol ether) (
nonylphenol 9.5-mole ethoxylate), Surfonic; N-120(nonylphenol 12-mole
ethoxylate), Surfonic N-150 (nonylphenol 15-moie ethoxylate), Surfonic
N-200 (nonylphenol 20-mole ethoxylate) , Surfonic N-300( nonylphenol
30-mole ethoxylate) , Surfonic N-400 nonylphenol 40-mole ethoxylate,
Surfonic LF-7 (Alkyl polyoxyalkylene ether) , Surfonic LF-17
(ethoxylated and propoxylated linear primary 12-14 carbon number
alcohol), Igepal CO-630 (nonylphenoxy
poly(ethyleneoxy)ethanol,branched), Surfonic DNP-40
(dinonylphenol ethoxylate glycol ether).
6. A formulation as claimed in claim 1, wherein the preferred HLB value of the surfactant is between 16 and 40.
7. A formulation as claimed in claim 1, wherein the average mean size of the micro-reservoir is in the range of 5 nm to 2000 nm.
8. A perfumed acrylic fiber manufactured from a formulation as claimed in claim 1.
9. A perfumed acrylic yarn manufactured from a formulation as claimed in claim 1.
10. A perfumed acrylic fabric manufactured from a formulation as claimed in claim 1.
36

11. A process of preparation of a perfumed acrylic formulation meant for manufacture of acrylic products comprising the following steps :
• admixing a water-insoluble perfume constituent with a non-aqueous solvent, to form a non-aqueous phase ;
• heating the non-aqueous phase to a temperature in the range of 25°C to 95°C;
• dissolving and stirring a surfactant, optionally with a co-surfactant, a
solvent for acrylic polymer in water to obtain an aqueous phase;
• heating the aqueous phase;
• mixing the aqueous phase with the non-aqueous phase in liquid state to form an admixture, and homogenizing to obtain a micro-emulsion;
• mixing the micro-emulsion with an acrylic polymer solution in a solvent and water and further homogenizing and dispersing the micro-emulsion to obtain a polymer dope wherein the perfume constituent is embedded in evenly dispersed micro-reservoirs.
37
Dated this 3rd day of July, 2008


Documents:

1395-mum-2008-abstract.doc

1395-mum-2008-abstract.pdf

1395-MUM-2008-ANNEXURE TO FORM 3(26-9-2012).pdf

1395-MUM-2008-CLAIMS(AMENDED)-(26-9-2012).pdf

1395-MUM-2008-CLAIMS(AMENDED)-(28-2-2014).pdf

1395-MUM-2008-CLAIMS(MARKED COPY)-(28-2-2014).pdf

1395-mum-2008-claims.doc

1395-mum-2008-claims.pdf

1395-MUM-2008-CORRESPONDENCE(13-04-2010).pdf

1395-mum-2008-correspondence(18-7-2008).pdf

1395-MUM-2008-CORRESPONDENCE(24-7-2009).pdf

1395-mum-2008-correspondence.pdf

1395-mum-2008-description(complete).doc

1395-mum-2008-description(complete).pdf

1395-mum-2008-drawing.pdf

1395-MUM-2008-EP DOCUMENT(26-9-2012).pdf

1395-mum-2008-form 1(18-7-2008).pdf

1395-MUM-2008-FORM 1(28-2-2014).pdf

1395-mum-2008-form 1.pdf

1395-MUM-2008-FORM 18(24-7-2009).pdf

1395-mum-2008-form 2(titel page).pdf

1395-mum-2008-form 2.doc

1395-mum-2008-form 2.pdf

1395-MUM-2008-FORM 26(26-9-2012).pdf

1395-MUM-2008-FORM 3(13-04-2010).pdf

1395-mum-2008-form 3(3-7-2008).pdf

1395-mum-2008-form 3.pdf

1395-MUM-2008-MARKED COPY(26-9-2012).pdf

1395-MUM-2008-PETITION UNDER RULE-137(28-2-2014).pdf

1395-MUM-2008-REPLY TO EXAMINATION REPORT(26-9-2012).pdf

1395-MUM-2008-REPLY TO HEARING(28-2-2014).pdf

1395-MUM-2008-SPECIFICATION(AMENDED)-(26-9-2012).pdf

abstract1.jpg


Patent Number 259903
Indian Patent Application Number 1395/MUM/2008
PG Journal Number 14/2014
Publication Date 04-Apr-2014
Grant Date 28-Mar-2014
Date of Filing 03-Jul-2008
Name of Patentee ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD
Applicant Address ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI,
Inventors:
# Inventor's Name Inventor's Address
1 LODHA PREETI ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400025,
2 MAHAJAN TUSHAR ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400025,
3 KAPOOR BIR ADITYA BIRLA CENTRE, 2ND FLOOR, C WING, S.K. AHIRE MARG, MUMBAI-400025,
PCT International Classification Number D06M15/693,A41B11/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 1259/MUM/2007 2007-07-03 India