CLIAMS:We Claim:
1. An aqueous microcapsule suspension with enhanced stability, comprising:
- from 25 to 75 weight % of a microcapsule, the microcapsule comprising an aminoplast polymer shell and hydrophobic core material, the hydrophobic core material further comprising from 0 to 50 weight % of a water insoluble polyhydroxy compound and a remaining % weight of a single active or a plurality of actives of the total weight % of the microcapsule;
- from 0.01 to 10 weight % of a water soluble polyhydroxy compound;
- from 75 - 25 weight % of water; and
- the microcapsule additionally optionally comprising a cationic polymer coating.

2. The aqueous microcapsule suspension as claimed in claim 1, wherein the microcapsule capsule diameter varies from about 10 nanometres to about 200 microns, preferably from about 50 nanometers to about 100 microns and most preferably from about 2 to about 15 microns. 3. The aqueous microcapsule suspension as claimed in claim 1, wherein the water soluble polyhydroxy compound is present in a dispersed aqueous phase.
4. The aqueous microcapsule suspension as claimed in claim 1, wherein the water insoluble polyhydroxy compound is present inside the hydrophobic core material.
5. A final consumer product selected from a group consisting of fragrance, detergent powder, liquid detergent, fabric conditioner, fabric refresher, fabric softener, paint, mosquito repellents, antibacterial, antifungal, antimicrobial, thermochromic inks, fabric whitener, fabric dye, inks, phase change material Insect repellents, moth repellents, fragranced whitener, silicones, flame retardants, perfumes, polysiloxanes, colours, dyes, pigments, coolant compounds, and oil soluble active compounds comprising the aqueous microcapsule suspension as claimed in claim 1.
6. A process for producing an aqueous microcapsule suspension in a reactor, comprising the steps of:
- an aqueous solution containing a copolymer and deionised water; wherein the copolymer is selected from a group consisting of acrylic acid acrylamide copolymer solution, polyvinyl alcohol or acrylic acid terpolymers and mixtures thereof;
- adding to the above solution a precondensate after complete homogenization; wherein the precondensate is selected from a group consisting of melamine formaldehyde precondensates, urea formaldehyde precondensates or mixtures thereof; followed by constant stirring of the resultant solution;
- adding a mild organic acid drop wise till a pH of 4.5 is achieved, further maintaining a constant temperature at 25oC for a duration of one hour with stirring of the mixture;
- adding a core material and high shearing the resulting mixture to a mean droplet size of 2-15 microns; and
- cooling the resultant mixture for a duration of two hours till a off-white microcapsule suspension is obtained.
7. The process as claimed in claim 6, wherein the core material is selected from a group consisting of fragrance, antibacterial, antifungal, mosquito repellent, optical brighteners, softeners, silicones, flame retardants, inks, perfumes, polysiloxanes, colours, dyes, pigments, coolant compounds, pesticides, oil soluble active compounds and likes.
8. The process as claimed in claim 6, wherein the process optionally further comprises of coating of the microcapsule by a cationic polymer.
,TagSPECI:TITLE:

Aminoplast microcapsule suspension with enhanced stability and a method of preparation thereof.

FIELD OF INVENTION:

The present invention relates to the field of aminoplast capsules and more specifically an aminoplast microcapsule suspension with polyhydroxy compounds and a method of preparation thereof, as well as final products containing them. This microcapsule suspension provides controlled release of the encapsulated actives from the associated final products containing them alleviating premature release either during the manufacturing of the product containing them or with slightest shear after drying on various substrates such as fabric, hair or hard surfaces like paper, metal, polymers, etc.

BACKGROUND OF THE INVENTION:

The concept of Encapsulation of actives has been a widely accepted process across numerous industries because of the need of targeted delivery and controlled release of the actives or internal phase e.g. fragrances and is therefore undergoing constant research and innovation. Several techniques are prevalent in the state of the art to provide microcapsules containing actives like perfume, antibacterial, antifungal, mosquito repellent, softeners and other actives. US Patent 4396670 describes a process for production of microcapsules by polymerisation of melamine formaldehyde precondensate in an aqueous medium containing dispersed particles of liquid to be encapsulated. Another discussion of active encapsulation specifically fragrance encapsulation is found in Kirk Othmer Encyclopedia. Preferred encapsulating polymers include those formed from melamine-formaldehyde or urea-formaldehyde condensates, as well as similar types of aminoplasts. A representative process used for aminoplast encapsulation is disclosed in U.S. Pat. No. 4396670 though it is recognized that many variations with regard to materials and process steps are possible. Both of these processes are discussed in the context of fragrance encapsulation for use in consumer products in U.S. Patent Nos. 4,145,184 and 5,112,688 respectively.
The preparation of microcapsules typically involves forming a dispersion or emulsion of the fragrance in an aqueous solution of urea-formaldehyde or melamine formaldehyde pre-condensate and then causing condensation of the pre-condensate under acid catalysis conditions to produce microcapsules. Fragrance containing microcapsules of this type have been typically used in paper and cardboard applications, in "scratch & sniff' type products, as well as applied to textiles and other surfaces, wherein they release the perfume when the capsules are ruptured. In order to render such capsules more stable in media containing surfactant or softening agents, a large number of modifications to these basic aminoplast shells have been proposed in recent patent literature, namely by modifying the surface of the capsule via the use of a second polymer, in particular a cationic polymer. There are many prior art reports of the preparation of the microcapsules. In this context, particular reference is made here to the publications of Brown and White in J. Microencapsulation
The patent literature is also rich in examples of preparation of melamine-formaldehyde. U.S. Patent No. 4,396,670, describes in detail many preparation examples of capsules. In spite of enormous research and constant innovation in this field, stability and enhanced release characteristics seem to be a continuous concern apart from premature or untimely release of the actives.

SUMMARY OF THE INVENTION:

This summary is provided to introduce concepts related to aminoplast microcapsules suspension with enhanced stability and a method of preparation of the same and the concepts are further described below in the detailed description. This summary is not intended to identify essential features of the claimed subject matter nor is it intended for use in determining or limiting the scope of the claimed subject matter.
In one aspect of the invention, the present disclosure describes an aqueous microcapsule suspension with enhanced stability and release characteristics. The aqueous suspension comprises a microcapsule with a hydrophobic core and an aminoplast polymer shell. The suspension further comprises a water soluble or water insoluble polyhydroxy compound either in the free dispersed phase or inside the microcapsules, rendering the suspension enhanced stability.
In another aspect of the invention, a method of preparation of aminoplast microcapsule suspension has been provided.
In yet another aspect of the invention, final products essentially consumer or industrial products containing the aqueous microcapsule suspension has been provided. The microcapsule essentially encapsulate core materials or actives enabling targeted delivery and controlled release, the actives including but not limiting to fragrance, antibacterial, antifungal, mosquito repellent, optical brighteners, softeners, silicones, flame retardants, inks, perfumes, silicones, polysiloxanes, colours, dyes, pigments, coolant compounds, pesticides, oil soluble active compounds and likes.

BRIEF DESCRIPTION OF DRAWINGS

The detailed description is described with reference to the accompanying figures.
Figure 1 is representative of the evaluation of Fabric conditioner without cationic coating in terms of average intensity of fragrance with and without invention in support of Table 8.
Figure 2 is representative of the evaluation of Fabric conditioner with cationic coating in terms of average intensity of fragrance with and without invention in support of Table 9.
Figure 3 is representative of the evaluation of Detergent Powder without cationic coating in terms of average intensity of fragrance with and without invention in support of Table 10.
Figure 4 is representative of the evaluation of Detergent Powder with cationic coating in terms of average intensity of fragrance with and without invention in support of Table 11.
Figure 5a and 5b are micrographs of the microcapsule suspension without and with the invention respectively.
Figure 6 is representative of the average stability performance of the microcapsule suspension fragrance in powder detergent (before rubbing) with and without invention.
Figure 7 is representative of the average stability performance of the microcapsule suspension fragrance in powder detergent (after rubbing) with and without invention.

DETAILED DESCRIPTION:

The present disclosure relates to an aqueous aminoplast microcapsule suspension, a method of preparation thereof and final products containing the microcapsule suspension.
The aqueous aminoplast suspension comprises of the microcapsule, water soluble polyhydroxy compound and water content. The microcapsule further comprises of water insoluble polyhydroxy compounds, core actives and an aminoplast polymer shell, these carrier systems rendering the microcapsules with enhanced stability and better release characteristics.
A representative Microcapsule suspension of the invention comprising of:
- 25% to 75 % microcapsules including the weight of the core materials, the core material further comprising of 0 to 50 weight % of water insoluble poly-hydroxy compound and the remaining by active materials with respect to weight % of core material;
- 0.01 % to 10% water soluble polyhydroxy compounds; and
- 75% to 25 % water.
Patent literature of particular pertinence for the manufacture of the melamine capsules includes U.S. Pat. No. 3,516,941 and U.S. Pat. No. 4,976,961, U.S. Pat. Nos. 4,406,816 and 6,224,795, WO Patent 01/51197 or U.S. Pat. No. 6,719,931 (BASF) and U.S. Pat. No. 6,261,483, WO 98/28396 or U.S. Pat. No. 6,194,375, in particular.
It is also described in the prior art that cationic transfer agents drive the deposition of such aminoplast capsules on fabric, skin and hair. This is of particular importance when such aminoplast capsules are used in liquid rinse-off formulations like laundry detergents, fabric conditioners, shampoos, rinse-off hair conditioners and body washes.
In this context, U.S. Patent No. 4,234,627, , discloses a liquid fragrance coated with an aminoplast shell further coated by a water insoluble meltable cationic coating in order to improve the deposition of capsules from fabric conditioners. In U.S. Patent No. 4,973,422, from 1989, it was then further described that capsules with a cationic coating provide improved substantivity to the surface being treated, such as fabric treated with a fabric softener. The same idea was described in 1991 in U.S. Patent No. 5,185,155, where the selection of cationic polymers was enlarged to water soluble polymers and the type of encapsulation was distinct from those in the state of the art at the time. Patent application US 20040071742, discloses a similar technology where the fragranced aminoplast capsules are coated with cationic starch or cationic guar. International patent application WO 03/002699, describes fabric softening compositions where a cationic cross-linked polymer improves deposition of friable aminoplast microcapsules. The improved deposition of cationic microcapsules in rinse-off formulations is also generally disclosed in US Patent application 2003/0171246, and International patent application WO 01/62376, The descriptions of the nature and manufacture of all such microcapsules in these documents is hereby included by reference.
The present invention thus also includes coated aminoplast microcapsules prepared according to any of the methods described in these documents. Such "cationic coated" melamine fragrance microcapsules may be the result of the incorporation of classical melamine based capsules in products comprising cationic transfer agents, which will inevitably lead to stabilisation of the capsules by a cationic sort of coating surrounding the original uncoated melamine capsule, or may be prepared separately via the use of cationic polymers and then incorporated in the end product. The prior art cited here-above includes examples of both types of coated melamine microcapsules and the scope of the present invention extends to the use of all such examples of melamine formaldehyde or aminoplast based core and shell fragrance microcapsules.
Particle and capsule diameter can vary from about 10 nanometers to about 200 microns, preferably from about 50 nanometers to about 100 microns and most preferably from about 2 to about 15 microns. The capsule distribution can be narrow, broad, or multi-modal. Each modal of the multi-modal distributions may be composed of different types of capsule chemistries or capsule structures using different processing techniques.
Any suitable method for coating the cationically charged materials onto the encapsulated core materials can be used. After encapsulation, a cationically charged water-soluble or water dispersible polymer is applied to the microcapsules suspension. This water-soluble or dispersible polymer can also be an amphoteric polymer with a given ratio of cationic and anionic functionalities. The charge of these polymers can be adjusted by changing the pH, depending on the product in which this technology is to be used. The nature of suitable cationically charged polymers for assisted capsule delivery to interfaces depends on the compatibility with the capsule wall chemistry since there has to be some association to the capsule wall and that there should be no depletion reactions with the capsule wall structure.. This association can be made possible through physical interactions, such as hydrogen bonding, ionic interactions, hydrophobic interactions, electron transfer interactions. Therefore, depending on which capsule chemistry and interface (e.g. cotton, polyester, hair, skin, wool or mixtures of thereof) is used, the cationic polymer can be selected from one or more polymers with an overall zero or net positive charge, based on the following polymer backbones: polyurethane, polyoxazoline, polyamine, silicone, polyphosphazine, olyaromatic, poly heterocyclic, polysaccharides, polypeptides, polycarbonates, polyesters, polyolefinic polyester, polyether, or polyionene, comprising of vinyl, acrylic, acrylamide, poly-diene functions. As used herein molecular weight is provided as weight average molecular weight. Through loose coacervate / coating formation, these cationic or amphoteric polymers can be used in combination with nonionic and anionic polymers and surfactants to make required charge of cationic coating either zero or net positive depending on the formulation where the capsules are going in the final application.
Furthermore, it has been found that the compounds containing two or more than two hydroxyl functional group, forming an essential part of the microcapsule suspension, interact with the walls of the above aminoplast capsules in such a manner as to enhance their stability and retention capacity. These polyhydroxy compounds can be present inside the core or even outside the capsules and in the dispersed phase i.e. water medium and still exert their influence on the stability characteristics of such microcapsules. The only constraint on the choice of the polyhydroxy materials is that water soluble polyhydroxy materials should only be present in the dispersed aqueous phase and water insoluble hydrophobic polyhydroxy materials should only be present in the hydrophobic core of the microcapsules. These compounds exert their influence on the characteristics of the microcapsules even if they are present either before the cure / polymerisation of aminoplast shell or afterwards. Without wishing to be bound by theory it is postulated that the said polyhydroxyl compounds of this invention do not take part within the polymerisation reaction of the aminoplast pre polymer but by a mechanism similar to “plasticisation” of the final aminoplast polymer shell. Plasticisation is described by various people in various ways. One such description is given in Principles of Plasticization by EDMUND H. IMMERGUT and, HERMAN F. MARK, Polytechnic Institute of Brooklyn, Brooklyn, N. Y. as follows:
Plasticization, in general, refers to a change in the thermal and mechanical properties of a given polymer which involves: (a) lowering of rigidity at room temperature; (b) lowering of temperature, at which substantial deformations can be effected with not too large forces; (c) increase of the elongation to break at room temperature; (d) increase of the toughness (impact strength) down to the lowest temperature of serviceability. These effects can be achieved: (1) by compounding the given polymer with a low molecular weight compound or with another polymers and (2) by introducing into the original polymer, a co-monomer which reduces crystalzabillty and increases chain flexibility.
By way of the present disclosure, it has further been found that this effect can be quantified using a TI 900 Triboindenter and tested by using low load tip TI-047, 200um dia 900 conical tip, tested in displacement range of 2nm to 1000 nm with selecting equal size capsules from range of 5 - 10 Microns and measured in elastic zone (before plastic deformation) by the parameter of “stiffness”. Stiffness is described as the ‘rigidity of an object”. It is defined as the extent to which the object resists deformation under the influence of an applied force”.
Water soluble polyhydroxy materials for the purposes of this invention are defined as organic materials with two or more than two hydroxyl functional groups, which have a log P < 2.3. Such materials are to be added outside the microcapsules. If water soluble polyhydroxy materials are added along with the hydrophobic core these materials tend to diffuse out of the core during the process of curing and thus leave deformed walls and therefore compromised structural integrity as well as no real encapsulation of the core materials. This defeats the purpose of encapsulation and therefore it is avoided. Instead water soluble polyhydroxy materials are added to the fully formed microcapsules suspension (before a coating process). If a coating process is required on the capsules then the coating polymers are added to the microcapsule slurry after the mixtures of microcapsules and polyhydroxy water soluble materials have been formed and a minimum aging period is over.
Water in-soluble polyhydroxy materials for the purposes of this invention are organic materials with two or more than two hydroxyl functional groups, having logP > 2.3.These will be forming a part of the core materials which are encapsulated and hence these materials will typically be having the functionality of the other core materials e.g. aromachemicals, antibacterials, antifungals, pesticides, dyes, UV blockers etc but could also be other water insoluble materials added to the core for the sole purpose of giving the enhanced stability of microcapsules as per the invention.
This aqueous microcapsule suspension according to the invention can then further be dried to a dry powder form using known means such as spray drying, spin flash drying etc. to yield dry microcapsule powder of appropriate composition. A process for preparation of the microcapsules suspension is described herein. The present process may take place in a batch process but it can also be carried out in a continuous reactor specifically reactors with principally plug flow characteristics.
In a reactor, a copolymer solution is added to de-ionised water. After complete homogenization a precondensate is added. In this context, the copolymer solution can be selected from a group consisting of polymer solutions either singly or mixtures of acrylic acid acrylamide copolymer solution, Lupasol PA 140 , Alcapsol 144 (BASF), KEMIRA, polyvinyl alcohol or Acrylic acid terpolymers. The precondensate can be selected from a group consisting of melamine formaldehyde precondensates Or either singly or mixtures of resins such as CYMEL 303, 323, 327, 328, 385, P707 (Cytec), Or BC 336 (British Industrial Plastics) or Luracoll SD (BASF) or urea formaldehyde precondensates e.g. Cymel U60, U65 and UM15 . The resulting mixture is then stirred until a uniformly homogenous solution is obtained. Acetic acid or any other mild organic acid is then added drop wise till pH of 4.5 is reached. The mixture is stirred at constant temperature of 25ºC for a duration of one hour following which a core material is added and the mixture is high sheared through suitable means to a mean droplet size of 2-15 microns was reached. The core material comprises of a water soluble polyhydroxy compound and actives which are essentially encapsulated for stability and retention capacity. The core material in view of the actives which can be employed in this invention includes but is not limited to fragrance, antibacterial, antifungal, mosquito repellant, optical brighteners, softeners, silicones, flame retardants, inks, perfumes, silicones, polysiloxanes, colours, dyes & pigments, coolant compounds, pesticides and all oil soluble active compounds and the likes. Furthermore, the temperature is raised to 80ºC for 2 hours to cure the outer shell of microcapsule so formed. After 2 hours the mixture is cooled and an off-white slurry containing microcapsules in suspension is obtained. These capsules were coated with a Cationic polymer, an additional optional step by adding the cationic polymer drop wise to the capsule slurry under homogenization or adding the capsule slurry to a solution of cationic polymer in water drop wise till the desired quantities have been added together. The cationic polymers for coating the above capsule can be selected from a group consisting of cationic polymers either singly or mixtures of UCARE 30M Polyquaternium 10, Polyquaternium 11, Polyquqaternium 7, Salcaret SC 60, Cationic Guars like Jaguar® from Rhodia, Gluadin® WQT, Merquats ® , Eudragit ® RL30D, Rheovis® CDE, Luviquat® Care, Lupasol® P, Q2-7224 Dow Corning, 929 emulsion , ABIL® Quat 3270 Degussa, Tegopren 6924 Evonik.
In a typical composition according to the present disclosure made by the above process, the weight of the copolymer solution is from 1 to 20 weight % of the total weight of the suspension. The weight of the deionised water is 75 to 25 weight % of the total weight of the suspension. Furthermore, weight of the precondensate ranges from 5 - 89 weight % of the total weight of the suspension and the weight of the core material ranges from 10 - 90 weight % of the total weight of the suspension. The contributory range of the additional cationic polymer coating is from 1 -10 weight % of the total weight of the suspension.
The actives or core materials used in this invention include without limitation, any combination of active compounds, essential oil, plant extract or mixture thereof that is compatible with, and capable of being encapsulated by a polymer. Source of suitable active compounds is found in Perfumes Cosmetics and Soaps, Second Edition, edited by W. A. Poucher, 1959.Among the active compounds provided in this treatise are acacia, cassie, chypre, cylamen, fern, gardenia, hawthorn, heliotrope, honeysuckle, hyacinth, jasmine, lilac, lily, magnolia, mimosa, narcissus, freshly-cut hay, orange blossom, orchids, reseda, sweet pea, tuberose, vanilla, violet, wallflower, and the like.
Many types of actives or core materials can be employed in the present invention, the only limitation being the compatibility and ability to be encapsulated by the polymer being employed, and compatibility with the encapsulation process used. Suitable active compounds include but are not limited to fruit extracts or natural extracts such as extracts of almond, apple, cherry, grape, pear, pineapple, orange, strawberry, raspberry; musk, flower scents such as lavender like, rose-like, iris-like, and carnation-like. Other pleasant scents include herbal scents such as rosemary, thyme, and sage; and woodland scents derived from pine, spruce and other forest smells. The fragrances and aromas can here originate from a large number of plant starting materials for example from lavender, rose, jasmine, neroli; stems and leaves, for example from geranium, patchouli, petitgrain, fruits, such as anise, coriander, caraway, juniper; fruit peels, for example from citrus fruits, such as bergamots, lemons, oranges; seeds, such as mace, angelica, celery, cardamom; roots, such as angelica, cosus, iris, calmus; wood, such as sandalwood, guaiac wood, cedarwood, rosewood; herbs and grasses, such as tarragon, lemongrass, sage, thyme; needles and branches, for example from spruces, firs, pines, dwarf-pines; resins and balsams, for example from galvanum, elemi, benzoin, myrrh, olibanum, opoponax. Active compounds may also be derived from various oils, such as essential oils, or from plant materials such as peppermint, spearmint and the like. Other familiar and popular smells can also be employed such as baby powder, popcorn, pizza, cotton candy and the like in the present invention.
Typically, perfumes and fragrances are the complex mixtures of a plurality of organic compounds and the composition employed in the present invention, but are not limited to, hexyl cinnamic aldehyde; amyl cinnamic aldehyde; amyl salicylate; hexyl salicylate; terpineol; 3,7-dimethyl-c is-2,6-octadien-1-ol; 2,6-dimethyl-2-octanol; 2,6-dimethyl-7-octen-2-ol; 3,7-dimethyl-3-octanol; 3,7-dimethyl-t rans-2,6-octadien-1-ol; 3,7-dimethyl-6-octen-1-ol; 3,7-dimethyl-1-octanol; 2-methyl-3-(para-tert-butylphenyl)-propionaldehyde;4-(4-hydroxy-4-methylpentyl)-3-cyclohexene-1-carboxaldehyde; ricyclodecenyl propionate; tricyclodecenyl acetate; anisaldehyde; 2-methyl-2-(para-iso-propylphenyl)-propionaldehyde; ethyl-3-methyl-3-phenyl glycidate; 4-(para-hydroxyphenyl)-butan-2-one;1-(2,6,6-trimethyl-2-cyclohexen-1-yl)-2-buten-1-one; para-methoxyacetophenone; para-methoxy-alpha-phenylpropene;methyl-2-n-hexyl-3-oxo-cyclopentane carboxylate; undecalactone gamma, orange oil; lemon oil; grapefruit oil; bergamot oil; clove oil; dodecalactone gamma; methyl-2-(2-pentyl-3-oxo-cyclopentyl) acetate; beta-naphthol methylether; methylbeta-naphthylketone; coumarin; decylaldehyde; benzaldehyde; 4-tert-butylcyclohexyl acetate; alpha,alpha-dimethylphenethyl acetate; methylphenylcarbinyl acetate; Schiffs base of 4-(4-hydroxy-4-methylpentyl)-3-cyclohexene-1-carboxaldehyde and methyl anthranilate; cyclic ethyleneglycol diester of tridecandioic acid; 3,7-dimethyl-2,6-octadiene-1-nitrile; ionone gamma methyl; ionone alpha; ionone beta; petitgrain; methyl cedrylone; 7-acetyl-1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl-naphthalene; ionone methyl; methyl-1,6,10-trimethyl-2,5,9-cyclododecatrien-1-yl ketone; 7-acetyl-1,1,3,4,4,6-hexamethyl tetralin; 4-acetyl-6-tert-butyl-1,1-dimethyl indane; benzophenone; 6-acetyl-1,1,2,3,3,5-hexamethyl indane; 5-acetyl-3-isopropyl-1,1,2,6-tetramethyl indane; 1-dodecanal; 7-hydroxy-3,7-dimethyl octanal; 10-undecen-1-al; iso-hexenyl cyclohexyl carboxaldehyde; formyl tricyclodecan; cyclopentadecanolide; 16-hydroxy-9-hexadecenoic acid lactone; 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-gamma-2-benzopyrane; ambroxane; dodecahydro-3a,6,6,9a-tetramethylnaphtho-[2,1b]furan; cedrol; 5-(2,2,3-trimethylcyclopent-3-enyl)-3-methylpentan-2-ol; 2-ethyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol; caryophyllene alcohol; cedryl acetate; para-tert-butylcyclohexyl acetate;patchouli; olibanum resinoid; labdanum; vetivert; copaiba balsam; fir balsam; and condensation products of: hydroxycitronellal and methyl anthranilate; hydroxycitronellal and indol; phenyl acetaldehyde and indol; 4-(4-hydroxy-4-methyl pentyl)-3-cyclohexene-1-carboxaldehyde and methyl anthranilate,geraniol; geranyl acetate; linalool; linalyl acetate; tetrahydrolinalool; citronellol; citronellyl acetate; dihydromyrcenol; dihydromyrcenyl acetate; tetrahydromyrcenol; terpinyl acetate; nopol; nopylacetate; 2-phenylethanol; 2-phenylethyl acetate; benzyl alcohol; benzyl acetate; benzyl salicylate; benzyl benzoate; styrallyl acetate; dimethylbenzylcarbinol; trichloromethylphenylcarbinyl methylphenylcarbinyl acetate; isononyl acetate; vetiveryl acetate; vetiverol; 2-methyl-3-(p-tert-butylphenyl)-propanal; 2-methyl-3-(p-isopropylphenyl)-propanal; 3-(p-tertbutylphenyl)- propanal; 4-(4-methyl-3-pentenyl)-3-cyclohexenecarbaldehyde; 4-acetoxy-3-pentyltetrahydropyran; methyl dihydrojasmonate; 2-n-heptylcyclopentanone; 3-methyl-2-pentyl-cyclopentanone; n-decanal; n-dodecanal; 9-decenol-1; phenoxyethyl isobutyrate; phenylacetaldehyde dimethylacetal; phenylacetaldehyde diethylacetal; geranonitrile; citronellonitrile; cedryl acetal; 3-isocamphylcyclohexanol; cedryl methylether; isolongifolanone; aubepine nitrile; aubepine; heliotropine; eugenol; vanillin; diphenyl oxide; hydroxycitronellal ionones; methyl ionones; isomethyl ionomes; irones; cis-3-hexenol and esters thereof; indane musk fragrances; tetralin musk fragrances; isochroman musk fragrances; macrocyclic ketones; macrolactone musk fragrances; ethylene brassylate etc.
Some of the composition for antifungal, antibacterial employed in the present invention are Clioquinol, Haloprogin, Miconazole nitrate, Povidone-iodine, Tolnaftate, Undecylenic acid, calcium undecylenate, copper undecylenate, zinc undecylenate, Clotrimazole, Triclosan, Triclocarban/Trichlorocarbamide and PCMX/Chloroxylenol, N-fluorodichloromethylthio phthalimide, o-phenylphenol, bis(tributyltin)oxide, 2-(thiocyanomethylthio) benzthiazole, N,N-dimethyl-N'-phenyl(N'-fluorodichloromethylthio)-phthalimide, Al-N-nitroso-N-cyclohexyl hydroxylamine, Zn-2-pyridinethiol-1-oxide, diiodomethyl-p-torylsulfone, 2,4,4'-trichloro-2'-hydroxydiphenyl ether, etc.; bactericicides such as 1,2-benzisothiazoline-3-one, methylene bisthiocyanate, 2-methy-4-chloroisothiazoline-3-one, tetrahydro-3,5-dimethyl-2H-1,3,5-thiadiazine-2-thione, bisbromoacetoxyethane, 2-bromo-2-nitrobutane-1,3-diol, 2-bromo-2-bromomethylglutaronitrile, 2,2-dibromo-3-nitrilopropionamide, bis(tribromomethyl) sulfone, etc.; and insecticides such as O,O-dimethyl-O-(3-methyl-1,4-nitrophenyl) phosphorothioate (Fenitrothione), O,O-dimethyl-O-(3-methyl-4-methylthiophenyl)phosphorothioate (Fenthione), O-(2,2-dichlorovinyl)-O,O-dimethyl phosphate (Dichlorvor), O,O-dimethyl-O-(2-isopropyl-4-methyl-6-pyrimidinyl) phosphorothioate (Diazinone),O-2,4-dichlorophenyl-O-ethyl-5-propyl phosphorodithoate (Frothiofos), (E)-O-2-isopropoxycarbonyl-1,1-,methylvinyl-O-methyl-N-ethyl phosphoramidothioate(Propilanphos),O,O-dimethyl-O-(3,5,6-trichloro-2-pyridyl)phosphorothioate (Chlopyrifod-methyl), etc.
Some known antifungal composition that have been used in the coatings industry are: copper (II) 8-quinolinolate (CAS No. 10380-28-6); zinc-dimethyl dithiocarbamate (CAS No. 137-30-4); 2-mercaptobenzothiazole,tributyl tin benzoate (CAS No. 4342-36-3); bis tributyl tin salicylate (CAS No. 22330-14-9), tributyl tin oxide (CAS No. 56-35-9); parabens: ethyl parahydroxybenzoate (CAS No. 120-47-8), propyl parahydroxybenzoate (CAS No. 94-13-3) methyl parahydroxybenzoate (CAS No. 99-76-3) and butyl parahydroxybenzoate (CAS No. 94-26-8); methylenebis(thiocyanate) (CAS No. 6317-18-6); 1,2-benzisothiazoline-3-one (CAS No. 2634-33-5); 2-mercaptobenzo-thiazole (CAS No. 149-30-4); 5-chloro-2-methyl-3(2H)-isothiazolone (CAS No. 57373-19-0); 2-methyl-3(2H)-isothiazolone (CAS No. 57373-20-3); zinc 2-pyridinethiol-N-oxide (CAS No. 13463-41-7); tetra-hydro-3,5-di-methyl-2H-1,3,5-thiadiazine-2-thione (CAS No. 533-74-4); N-trichloromethyl-thio-4-cyclohexene-1,2-dicarboximide (CAS No. 133-06-2); 2-n-octyl-4-isothiazoline-3-one (CAS No. 26530-20-1); 2,4,5,6-tetrachloro-isophthalonitrile (CAS No. 1897-45-6); 3-iodo-2-propynyl butylcarbamate (CAS No. 55406-53-6); diiodomethyl-p-tolylsulfone (CAS No. 20018-09-1); N-(trichloromethyl-thio)phthalimide (CAS No. 133-07-3); potassium N-hydroxy-methyl-N-methyl-dithiocarbamate (CAS No. 51026-28-9); sodium 2-pyridinethiol-1-oxide (CAS No. 15922-78-8); 2-(thiocyanomethylthio) benzothiazole (CAS No. 21564-17-0); 2-4(-thiazolyl) benzimidazole (CAS No. 148-79-8) etc.
The various repellent compositions work effectively against arachnids (spiders, ticks, and mites), caterpillars, cockroaches, silver fish, moths, slugs, bees, yellow jackets, beetles, aphids, meal bugs, green flies, horse flies, gnats, mosquitoes, and chiggers. Repellent composition includes N,N-diethyl-m-toluamide(DEET), DDT, DETA, DEBA, DEPA, Picaridin, Permethrin, Icaridin, Salatine, some synthetic pyrethroids, methomyl, Phosmet, dimethyl dichlorovinyl phosphate (DDVP), chlorpyrofos, N,N-diethylbenzamide; citronella; Tolu balsam; Peru balsam; Eucalyptus oil; Huon pine oil; camphor; cypress oil; galbanum; diethyl phthalate; dimethyl phthalate; dibutyl phthalate; butanal; 1-ethoxy-1-(2'-phenylethoxy)ethane; acetyl cedrene, propylidene phthalide and the like.
Examples of the bactericides, but are not necessarily limited to, glutaraldehyde, formaldehyde, 2-bromo-2-nitro-propane-1,3-diol, a mixture of 5-chloro-2-methyl-4-isothiazoline-3-one and 2-methyl-4-isothiazoline-3-one etc.
Optical brighteners can be employed in the present invention are commercially available which can be classified into subgroups, which include, but are not necessarily limited to, derivatives of stilbene, pyrazoline, coumarin, carboxylic acid, methinecyanines, dibenzothiophene-5,5-dioxide, azoles, 5- and 6-membered-ring heterocycles and other miscellaneous agents. Examples of these types of brighteners are disclosed in "The Production and Application of Fluorescent Brightening Agents", M. Zahradnik, Published by John Wiley & Sons, New York (1982), and can be make stable by this invention for control release in application. Dyes and pigments can be employed in the present invention, Organic dyes and pigments are well known products, described and classified in many reference books, among which may be mentioned Lubs, The Chemistry of Synthetic Dyes and Pigments (Reinhold Publishing Corp, 1955), and Pratt, Chemistry and Physics of Organic Pigments (John Wiley & Sons, 1947). From the chemical standpoint, they belong to a variety of classes, the principal ones of which are listed below for reference. With each class is shown, by way of illustration, one or more representative examples of technically important dyes and pigments of that class. These specific dyes and pigments are listed under the names and reference numbers used in the Color Index, 2nd ed. (1956) are Thiazine, e.g, Basic Blue 9, Thiazole, e.g, Direct Yellow 28, Basic Yellow 1, Triarylmethanes, e.g, Basic Green 4, Alkali Blue 110, Xanthene, e.g, Acid Red 87, Pigment Red 81, Basic Violet 10, Sulfur Dyes, e.g, Sulfur Blue 7, Sulfur Red 1, Anthraquinone, e.g, Acid Blue 45, Acid Blue 78, Mor dant Violet 26, Vat Yellow 2, Vat Orange 9, Vat Black 27, Vat Blue 6, Indigoid, e.g, Vat Blue 5, Vat Violet 4, Vat Red 41, Vat Red 45, Phthalocyanine, e.g, Pigment Blue 15, Pigment Blue 17, Direct Blue 86, Quinacridone, e.g, the quinacridone pigments, A20, e.g, Direct Red 28, Direct Green 6, Acid Yellow 23, Disperse Yellow 3, Mordant Black 17, Pigment Red 1, Pigment Red 18, Pigment Red 50, Pigment Red 57, Acridine, e.g, Basic Orange 14, Azine, e.g, Basic Red 2, Solvent Black 5, Ketone imine, e.g, Basic Yellow 2, Methine, e.g, Disperse Yellow 31, Basic Yelow 11, Nitro, e.g, Acid Yellow 1, Pigment Yellow 11, Disperse Yellow 1, Nitroso, e.g, Acid Green 1, Oxazine, e.g, Basic Blue 12, Direct Blue 109,Quinoline, e.g, Acid Yellow 3, and mixtures of these pigments. There are so many manufacturers and supplier of silicone oils in India and abroad. Well-known manufaturers like Dow Corning, Hach company, Elkaysilicones, Khemocraft, mrsilicone, supremesilcones, mccoygroup, the silicone oils which can be employed in the present invention, but are not limiting to, Silicone Oils/Fluids, Silicone Antifoams, Silicone Emulsions, Epoxy Silicone Fluids, Carboxy Silicone Fluids, Amino Silicone Fluids, Simethicone I.P./ USP, Activated Dimethicone I.P, Speciality Silicone products like hard coatings, spinning sprays, metal degreaser, paper coatings, polymer coatings, silicone release coatings, silicone adhesives and likes. UV protection agents consists of active ingredients like avobenzone or a benzophenone such as dioxybenzone, oxybenzone, or sulisobenzone, Aminobenzoic acid (PABA), Cinoxate, Ecamsule, Homosalate, vobenzone, Menthyl anthranilate, Octocrylene, Octyl methoxycinnamate, Octyl salicylate, Oxybenzone, Padimate O, Phenylbenzimidazole, Sulisobenzone, Trolamine salicylate, Octyl methoxycinnamate, 4-methyl benzylidine camphor, Homosalate, and combinations thereof.
Suitable physiological cooling agents that are preferred in this aspect of the invention are menthyl succinate; menthyl lactate; 3-l-menthoxypropane-1,2-diol; menthone glycerol ketals; N-substituted p-menthane carboxamide; acyclic carboxamide and mixtures thereof, N-substituted p-menthane carboxamide (WS-3), acyclic carboxamide (WS-23) and menthyl lactate. menthyl succinate; acyclic carboxamide; menthyl lactate; 3-l-menthoxypropane-1,2-diol; N-substituted p-menthane carboxamide, hydroxymethyl and hydroxyethyl derivatives of p-menthane, 2-mercapto-cyclo-decanone, methylcyclohexanol, hydroxycarboxylic acids with 2-6 carbon atoms, menthone glycerol ketals, 3-l-menthoxypropane-1,2-diol, menthyl lactate, menthone glycerol ketal (MGK), menthyl lactate (ML), menthyl succinate (MS), 3-l-menthoxypropane-1,2-diol (TCA), acyclic carboxamides (AC), substituted p-menthane carboxamides (PMC) and the mixture thereof.
Some examples of water soluble polyhydroxy materials without limitation to be added to the dispersed aqueous phase are as follows:
Fragrance:
Table 1: Water soluble polyhydroxy fragrance compounds
Compound name CAS no.
Argireline 616204-22-9

Dipropylene glycol 110-98-5
Diethylene glycol monomethyl ether 111-77-3
2,5-Dimethyl-2,5-dihydroxy-1,4-dithiane 55704-78-4
Vanillin propylene glycol acetal 68527-74-2
Guaiacol 90-05-1
Sorbitol 50-70-4
Mannitol 69-65-8
Glucuronolactone 32449-92-6
2,5-Dihydroxy-1,4-dithiane 40018-26-6

4 hydroxy phenyl ethyl alcohol 501-94-0
Vanillyl alcohol 498-00-0
p coumaryl alcohol 3690.05.9
4 hydroxy benzyl alcohols 623-05-2

Propylene Glycol 57-55-6
Ethylene Glycol 107-21-1
Glycerol 56-81-5
Glycerol monostearate 31566-31-1

Insecticides & Pesticides:
Table 2: Water soluble polyhydroxy insecticide and pesticide compounds
Compound name CAS no.
Erythritol 10030-58-7
Catechol (also in castoreum) 120-80-9

Others like cosmetic agents, Coolants,Natural exract & Buffering Agents:
Table 3: Water soluble polyhydroxy compounds
Compound name CAS no.
3-O-Ethyl-L-ascorbic acid 86404-04-8

alpha-Arbutin 84380-01-8

Pentaerythritol 115-77-5

Rosmarinic acid 20283-92-5

2-Methyl-2,4-pentandiol 107-41-5
1,3-Benzenediol, 4-(2-phenyldiazenyl)- 2051-85-6
Neohesperidin dihydrochalcone 20702-77-6
2-Amino-2-(hydroxymethyl)-1,3-propanediol 77-86-1
Monoglycol salicylate 87-28-5
Benzenemethanol,2-hydroxy- 90-01-7

4-methylcatechol 452-86-8

Agnuside 11027-63-7

Ribitol 488-81-3
Orcinol 504-15-4
5-hydroxy maltol 1073-96-7
Hydroxydihydromaltol 28564-83-2

coniferyl alcohol 458-35-5
Water insoluble polyhydroxy materials are to be added inside the microcapsule core
Some example of water insoluble polyhydroxy materials without limitations to be added inside the microcapsule core are as follows:
Fragrance:
Table 4: Water insoluble polyhydroxy fragrance compounds
Compound name CAS no.
1,3-Nonanediol acetate (mixed esters) 1322-17-4
3-l-Menthoxypropane-1,2-diol 87061-04-9

4-Ethyl-6-(2,6,6-trimethylyclohex-2-en-1-yl)hex-2-ene-1,4-diol, 90411-73-7
Oils, jasmine, Jasminum sambac 1034798-23-6
Decahydro-beta-naphthyl acetate 10519-11-6
Hydroxycitronellol 107-74-4
Dihydromyrcenyl acetate 53767-93-4
Octadecanoic acid, monoester with 1,2,3-propanetriol 31566-31-1
Atranorin 479-20-9
ChloroAtranorin 479-16-3
Alectorialic Acid 28789-23-3
Emodin 518-82-1
7-ChloroEmodin 18521-72-7
Chrysophanol 481-74-3
Sorbitan esters 9005-64-5
Tannins 1401-55-4

Citral propylene glycol acetal 10444-50-5
Oils, Callitropsis nootkatensis 1069136-34-0
Heptaldehyde, ethylene glycol acetal 1708-34-5
Vanillin 3-(l -menthoxy)propane-1,2-diol acetal 180964-47-0
9,10-Anthracenedione, 1,4-bis[(4-butylphenyl)amino]-5,8-dihydroxy- 28198-05-2
Methyl 2,4-dihydroxy-m-toluate 33662-58-7
Ethyl vanillin propylene glycol acetal 68527-76-4
Deertongue leaf incolore 68606-82-6
5,5'-(1-Methylethylidene)bis[1,1'-(bisphenyl)-2-ol] 24038-68-4
Sclareol 515-03-7
(Evernyl) Methyl 2,4-dihydroxy-3,6-dimethylbenzoate 4707-47-5
bis(dihydroxypropyl)dimethylammonium chloride 40509-16-8


Insecticides & Pesticides:
Table 5: Water insoluble polyhydroxy insecticide and pesticide compounds
Compound name CAS no.
Abamectin 71751-41-2
Usnic Acid 125-46-2
Hypericin 548-04-9
VioXanthin 15447-05-9
Polyporic Acid 548-59-4
p-Menthane-3,8-diol 42822-86-6
Amphidinol 132930-70-2
Others like cosmetic agents, Coloring agents, Coolants, Natural extract & Buffering agents:
Table 6: Water insoluble polyhydroxy other compounds
Compound name CAS no.
1,10-Decanediol 112-47-0
2,7-Naphthalenediol 582-17-2
1,3-Benzenediol, 4-(2-phenyldiazenyl)- 2051-85-6
4-tert-Butylcatechol 98-29-3
Zeaxanthin 144-68-3
Stictic Acid 549-06-4
Norstictic Acid 571-67-5
Lobaric Acid 522-53-2
FumarProtoCentraric Acid 489-50-9

Lecanoric Acid
480-56-8
Evernic Acid 537-09-7
Gyrophoric Acid 548-89-0
8 hydroxy linalool 103619-06-3
8 hydroxy geraniol 26488-97-1
1,10-Decanediol 112-47-0
2-oleamido-1,3-Octadecanediol 54422-45-6
(2,3-Dihydroxypropyl)stearat 123-94-4
1,3,5-Trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene 1709-70-2
Sebacic acid 111-20-6
Hydroxypropyl methylcellulose phthalate 9050-31-1
3-Octade-Canediol 764-22-7
ProtoCetraric Acid 489-51-0
Diffractaic Acid 436-32-8
Parietinic Acid
17636-18-9
Zeorin 22570-53-2
Glcyerol monostearate 31566-31-1
gallotannic acid 61790-06-5
Resin acids and rosin acids, hydrogenated, esters with triethylene glycol 68648-53-3
1,2-Octanediol 1117-86-8

Glyceryl monoricinoleate 1323-38-2

Resveratrol 501-36-0

7-Ethyl-10-hydroxycamptothecin 86639-52-3

Chrysin 480-40-0
Kaempferide 491-54-3

Examples
Examples and comparative examples of the present invention will be illustrated below, but the present invention is not limited to them.
Example 1: Relative stiffness and hardness of capsules
Anionic melamine formaldehyde capsules containing liquid fragrance Baby Soft from Tanishka Products Mumbai were prepared following the procedure described above. One part of this capsules slurry thus obtained was isolated for further testing (Microcapsule Slurry A) and separately to another part of this slurry was added 2% Glycerine IP grade and mixed well using a paddle mixer. The resulting mixture was left undisturbed for 48 hours (Microcapsule Slurry B). Samples of this mixture and the isolated unmodified slurry were then applied on cloth and also taken up for nanoindenter testing as described below
Nano-indenter used: TI 900 TriboIndenter from Hysitron, Minneapolis USA, model TI 900 using low load tip TI-047, 200um dia 900 conical tip, tested in displacement range of 2nm to 1000 nm.
The above samples described herein and henceforth were mounted on glass slides using a dilute solution of film forming polymer and air dried at 45 degree Celsius using a hand held dryer.
Measurements were taken in the elastic zone (before plastic deformation) after selecting roughly equal size capsules in the range of 5-10 microns.

Table 7: Nanoindentation reading for stiffness and hardness
Parameters Microcapsule A Microcapsule B
Avg Stiffness (?N/nm) 75 148
Avg Hardness (GPa) 0.875 1.89
Thus it shows that microcapsule slurry prepared in the manner of this invention had higher stiffness and hardness readings thus making them more stable to shear forces normally experienced in various product formats during manufacture, storage and application as well as during the actual trigger phase of the capsules while being used in their various applications on fabric, hair, skin and hard contact surfaces like metal, polymer or concrete etc.
Example 2: Exudation of phase change material (PCM)
Anionic melamine formaldehyde capsules containing liquid Phase change material (PCM) OM21 from Pluss Polymer News Delhi were prepared following the procedure described above. One part of this capsules slurry thus obtained was isolated for further testing and separtely to another part of this slurry was added 2% Ethylene Glycol LR Grade and mixed well using a paddle mixer. The resulting mixture was left undisturbed for 48 hours. Samples of this mixture and isolated unmodified slurry were then tested as per the following procedure.
Anionic microcapsules containing PCM were retrieved from both the above slurries by centrifuging them in a slightly acidic medium and drying the precipitate in oven @100 C for 2 hours. Then the recovered microcapsules were spread in a thick layer 1 cm thick on pre weighed Whatman Filter paper at a temperature of 100?C in an constant temperature oven. 2 kg standard load were kept on this layer of recovered microcapsules and observed for exudation. Exudation if any was measured by weighing the filter again and noting down the gain in weight.
Results – without polyhydroxyl compound - 10.5% exudation
With polyhydroxyl compound - 1.9% exudation
Thus anionic microcapsules containing PCM in the manner of this invention were demonstrated to have better stability.
Example 3: Olfactive evaluation in Fabric conditioners
Anionic melamine formaldehyde capsules containing fragrances named Baby Soft, Green Fruits and Spring Clean from Tanishka Products Mumbai with and without cationic coating are evaluated for with and without invention.
Washing conditions - Machine Samsung top load diamond drum, Delicate wash, level 1, 220g Terry Towel, 60 g Detergent powder , 60 g Fabric conditioner , 100 ppm Water hardness, Wash temperature of 270 C
Olfactory evaluation by 6 trained panellists, Assessment is made 2 hours after rinse (wet towels) and after 1 day, before and after gentle rubbing
Intensity scale is 0 = Not perceivable, 1= Very weak perceivable, 2 = Perceivable, 3 = Moderate perceivable, 4 = Strong perceivable, 5 = Very strong perceivable

Table 8: without Cationic Coating for Fabric conditioner evaluation

Average Intensity of Fragrance
Fabric conditioner Fragrance Baby Soft without Invention Fragrance Baby Soft
with Invention Fragrances Green Fruit without Invention Fragrances Green Fruit
with Invention Fragrance Spring Clean without Invention Fragrance Spring Clean
with Invention
After rinse
2 hrs in wet 3.1 3.2 3.2 3.2 3.2 3.2
24 hrs
before rubbing 3.3 3.7 3.2 3.5 3.3 3.7
24 hrs
After rubbing 4.7 5.0 4.6 5.0 4.3 4.9
The results of the above table are represented in Figure 1.
Table 9: with Cationic Coating for Fabric conditioner evaluation
Average Intensity of Fragrance
Fabric
conditioner Fragrance Baby Soft
without Invention Fragrance Baby Soft
with Invention Fragrance Green Fruit without Invention Fragrance Green Fruit
with Invention Fragrance Spring Clean without Invention Fragrance Spring Clean with Invention
After rinse
2 hrs in wet 2.9 3.4 3.3 3.3 3.3 3.4
24 hrs
before rubbing 3.2 3.8 3.4 3.4 3.4 3.8
24 hrs
After rubbing 4.3 4.9 4.7 5.0 4.4 5.0
The results of the above table have been represented in Figure 2.
Hedonic acceptance has not been done as it is related to perfume character which is not part of this investigation
Example 4: Olfactive evaluation in detergent powder
Anionic melamine formaldehyde capsules containing fragrance of Baby Soft, Green Fruits and Jade Fresh from Tanishka Products Mumbai with and without cationic coating are evaluated in non-perfumed detergent powder at 0.2 % dosage with and without invention.
Washing conditions - Machine Samsung top load diamond drum, Delicate wash, level 1, 220g Terry Towel, 60 g Detergent powder , 100 ppm Water hardness, Wash temperature of 270C.
Olfactory evaluation by 6 trained panellists, Assessment is made 2 hours after rinse (wet towels) and after 1 day, before and after gentle rubbing
Intensity scale is 0 = Not perceivable, 1= Very weak perceivable, 2 = Perceivable, 3 = Moderate perceivable, 4 = Strong perceivable, 5 = Very strong perceivable
Table 10: without cationic coating for Detergent powder evaluation
Average Intensity of Fragrance
Detergent powder Fragrance Baby Soft
without Invention Fragrance Baby Soft
with Invention Fragrance Green Fruit without Invention Fragrance Green Fruit with Invention Fragrance Jade Fresh
without Invention Fragrance Jade Fresh
with Invention
After rinse 2 hrs in wet 3.2 3.3 3.1 3.2 3.3 3.3
24 hrs
before rubbing 3.2 3.5 3.1 3.5 3.3 3.6
24 hrs
After rubbing 4.3 4.8 4.3 4.9 4.3 4.8
The results of the above table have been represented in Figure 3.
Table 11: with cationic coating for Detergent powder evaluation
Average Intensity of Fragrance
Detergent powder Fragrance Baby Soft
without Invention Fragrance Baby Soft
with Invention Fragrance Green Fruit
without Invention Fragrance Green Fruit
with Invention Fragrance Jade Fresh
without Invention Fragrance Jade Fresh
with Invention
After rinse 2 hrs in wet 3.2 3.4 3.4 3.4 3.5 3.4
24hrs before rubbing 3.4 3.8 3.3 3.5 3.8 4.1
24 hrs
After rubbing 4.5 5.0 4.8 5.0 4.7 5.0
The results of the above table have been represented in Figure 4.
Hedonic acceptance not done as it is related to perfume character which is not part of this investigation
Example 5: Optical Micrograph evaluation
Slurry of microcapsules containing fragrance Green Lime Citrus from Tanishka products Mumbai with and without invention were diluted with deionised water and observed under Trinocular Biological Microscope. We have found that the capsules with the invention are uniform round structures as compared to capsules without invention as seen in Figure 5a and 5b. The capsules without invention having dents and hence are not uniform. It is postulated that the capsule walls strucutre in the invention behave differently from those without invention and this leads to the above observation where the dents are formed in the most brittle and unstable capsules . Thus this observation proves the invention helps in manufacturing stable capsules with better wall structure.
Example 6: Stability Performance Testing
Refers to resistance to premature release when dry during product storage specifically in response to shear forces experienced by the capsules when deposited on any surface e.g. skin, fabrics, hair or hard surfaces including paper, metal, polymer, stone or concrete substrates.
Fragranced capsules suspension of Fragrance green lime citrus (GLC) made by the above method with and without invention are mixed in standard non perfumed detergent powder base at 0.2 % level. Detergent Powder is shaken in a laboratory mixer, Horizontal mixer RM10W-80V CAT at 60 RPM for 4 hrs and then keep into stability chamber at 370 C -70%RH conditions for 1 week, 3 week, 6 week , 9 week and 12 week checked intensity of fragrance after washing for each interval of time.
Washing conditions - Machine Samsung top load diamond drum, Delicate wash, level 1, 220g Terry Towel, 60 g Detergent powder , 100 ppm Water hardness, Wash temperature of 270C
Olfactory evaluation by 6 trained panellists, Assessment is made after 1 day line drying, before and after gentle rubbing
Intensity scale is 0 = Not perceivable, 1= Very weak perceivable, 2 = Perceivable, 3 = Moderate perceivable, 4 = Strong perceivable, 5 = Very strong perceivable
Table 12: Average stability performance for microcapsule suspension GLC in powder detergent before rubbing
Avrg. stability performance for microcapsule suspension GLC in powder detergent before rubbing (Intensity)
Microcapsule suspension GLC Initial 1 week 3 week 6 week 9 week 12 week
Without Invention 3.3 3.2 3.6 3.5 3.1 3.3
With Invention 3.4 3.3 3.5 3.5 3.3 3.6
The results of the above table have been tabulated in Figure 6.
Table 13: Average stability performance for Microcapsule suspension GLC in powder detergent after rubbing
Average stability performance for GLC in powder detergent after rubbing (Intensity)
Microcapsule GLC Initial 1 week 3 week 6 week 9 week 12 week
Without Invention 4.7 4.5 4.7 4.5 3.9 3.8
With Invention 5.0 4.9 4.9 4.8 4.5 4.3
The results of the above table have been represented in Figure 7.
Example 7: Mosquito repellent textile preparation and testing
There are many ways to applicate capsules on fabric surface like exhaust, padding, spraying, dip and dry etc. Anionic melamine formaldehyde capsules containing mosquito repellents with and without invention is applied to the fabric surface with padding method to untreated fabric of 100% cotton and 100% polyester to deposit 3.5 % of microcapsule suspension of permethrin (mosquito repellent) on dry weight of fabric. The fabrics applied with mosquito repellents are then cured at 1300 C. These cured fabrics are then washed with market detergent powder for continuous cycles of 10, 20, and 30 cycles.
Washing conditions - Samsung top load diamond drum, delicate wash, level 1, microcapsule suspension of permethrin (mosquito repellent) applied on 4 swatches of 100% cotton fabric and 4 swatches of 100% polyester fabric, 60 g detergent powder, 100 ppm water hardness, wash temperature of 270C.
After each 10 cycles one fabric of cotton and one fabric of polyester are removed and line dry for a day to dry fabric completely. These fabrics of cotton and polyester after wash are tested for mosquito repellence tests by taking 4 numbers of mosquitoes and are tested against applicated fabric (unwashed) and wash fabrics.
The microcapsule suspension made with invention are shown better repellence for mosquitoes as compare to the suspension made without invention and also gives knockdown(KD) in less time as compare to without invention. Results are tabulated below
Table 14: Mosquito repellence and knockdown (KD) results for capsules with & without invention
Sr. No. Fabric Type Original Fabric
(Unwashed) 10 washes 20 Washes 30 Washes
Without
Invention With
Invention Without
Invention With
Invention Without
Invention With
Invention Without
Invention With
Invention
1 Cotton KD in
30 min KD in
25 min KD in
120 min KD in
120 min KD in
70 min KD in
60 min KD in
210 min KD in
200 min
2 Polyester KD in
25 min KD in
20 min KD in
90 min KD in
80 min KD in 90min KD in
85 min KD in
210 min KD in
190 min
It is observed at the time of testing, mosquitoes are deactivates faster on fabric coated with mosquito repellent capsules with invention as compared to without invention. Overall, the time required to knockdown all mosquitoes is less in with invention compare to without invention, it shows the performance and hence stability of capsules containing permethrin actives (moquito repellant) as core. It is postulated that the invention helps in stabilizing the capsules on the fabric surface even under stressful conditions of multiple washes
Example 8: Antibacterial for Scrubs.
Anionic melamine formaldehyde capsules containing antibacterial actives with and without invention are applied to the scrubs. These scrubs are tested against an assessment of antibacterial activity by AATCC 147- 2011 method, with Test inoculums: Staphylococcus aureus ATCC 6538 and Klebsiella pneumoniae ATCC 4352 for Initial day and after 1 weak of use. Capsules with the invented method provide better diffusible antibacterial activity for scrubs in initial use and also for after one week use of scrub as compare to capsules without invention. Log reduction of bacteria count is more with invention than without invention.
Having hereby disclosed the subject matter of the present invention, it should be apparent that many modifications, substitutions, and variations of the present invention are possible in light thereof. As this technique covers areas in very vast fields like textile surfaces, paints and coatings, consumer goods and pesticides, it is understood that only some illustrative non limiting examples have been portrayed. It is to be understood that the present invention can be practiced other than as specifically described. Such modifications, substitutions and variations are intended to be within the scope of the present application.