Abstract: ABSTRACT A WAX INCORPORATED FRAGRANCE EMULSION COMPOSITION AND A PROCESS FOR ITS PREPARATION The present disclosure relates to a wax incorporated fragrance emulsion composition. Further, the present disclosure relates to a process for preparing the wax incorporated fragrance emulsion composition. The wax incorporated fragrance emulsion composition of the present disclosure is used to provide the long lasting effect of fragrance in the interior paint, and has mechanical, freeze-thaw, and accelerated storage stability for comparatively longer period of time.
Claims:WE CLAIM:
1. A wax incorporated fragrance emulsion composition comprising:
(i) a wax incorporated fragrance having a ratio of wax to fragrance is in the range of 1:8 to 1:40 by weight;
(ii) a layer of at least one copolymer;
(iii) at least one emulsifier;
(iv) at least one preservative;
(v) at least one neutralizer; and
(vi) q.s water.
2. The composition as claimed in claim 1, wherein a solid content is in the range of 40 to 50 wt% with respect to the total weight of the composition.
3. The composition as claimed in claim 1, wherein said wax is at least one selected from a paraffin wax and a Licocare® RBW 102 FL (renewable wax).
4. The composition as claimed in claim 1, wherein said fragrance is Muguet fragrance.
5. The composition as claimed in claim 1, wherein the composition is in the form of particles having a size in the range of 100 to 300 nm.
6. The composition as claimed in claim 1, wherein said copolymer is prepared by using a monomer selected from methyl methacrylate (MMA), methacrylic acid (MAA), 1,4-butanediol dimethacrylate (BDDMA), methacrylamide, and a combination thereof.
7. The composition as claimed in claim 1, wherein said copolymer is prepared by using methyl methacrylate (MMA) in an amount in the range of 90 to 93 wt. % with respect to total weight of monomers, methacrylic acid (MAA) in an amount in the range of 1 to 4 wt. % with respect to total weight of monomers, 1, 4-butanediol dimethacrylate (BDDMA) in an amount in the range of 0.5 to 1 wt. % with respect to total weight of monomers, and methacrylamide (20 wt% aq. solution) in an amount in the range of 3 to 8 wt. % with respect to total weight of monomers.
8. The composition as claimed in claim 1, wherein said emulsifier is selected from the group consisting of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), secondary alcohol ethoxylate (Tergitol 15 S 40), sodium lauryl sulfate (SLS), alkyldiphenyloxide disulfonate (Dowfax 2A1), polyoxyethylene tridecyl ether phosphate, ammonium salt (Rhodafac 610/A25), alcohol ethoxylates (ATPOL E5731/70N), and a combination thereof.
9. The composition as claimed in claim 1, wherein said preservative is selected from 5-Chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one (Kathon LX 150), monovalent salts of chloro-methyl, methyl isothiazolinone, and a combination thereof.
10. The composition as claimed in claim 1, wherein said neutralizer is selected from 2-amino-2-methyl-1-propanol (Amp-95), monoethanolamine and a combination thereof.
11. A process for preparing a wax incorporated fragrance emulsion composition, said process comprising the following steps:
a) mixing a predetermined amount of a wax and a fragrance at a first predetermined temperature for a first predetermined time period to obtain a homogeneous mixture;
b) adding a first predetermined amount of at least one emulsifier to the homogeneous mixture, followed by adding a demineralized water to obtain a second mixture;
c) adding a predetermined amount of a first mixture of monomers to the second mixture to obtain a third mixture;
d) adding a first predetermined amount of at least one initiator and a predetermined amount of a buffer solution to the third mixture at a second predetermined temperature and maintaining said second predetermined temperature for a second predetermined time period to obtain a fourth mixture;
e) adding a second predetermined amount of said emulsifier, a second predetermined amount of said initiator, and either a predetermined amount of second mixture of monomers or a predetermined amount of a pre-emulsion to the fourth mixture for a third predetermined time period to obtain a fifth mixture; and
f) mixing a predetermined amount of a chaser catalyst to said fifth mixture, followed by adding a neutralizer and a preservative to obtain said wax incorporated fragrance emulsion composition.
12. The process as claimed in claim 11, wherein said pre-emulsion is prepared by mixing a predetermined amount of at least one said emulsifier, a predetermined amount of said initiator, and a predetermined amount of at least one said monomer.
13. The process as claimed in claim 11, wherein said pre-emulsion in step e) comprises wax or fragrance or both.
14. The process as claimed in claim 11, wherein step e) is repeated up to three times to obtain wax incorporated fragrance emulsion composition with multiple shells.
16. The process as claimed in claim 11, wherein the first predetermined amount of at least one emulsifier is in the range of 1 to 4 wt. % with respect to the total weight of the composition and the second predetermined amount of at least one emulsifier is in the range of 1 to 3 wt. % with respect to the total weight of the composition.
17. The process as claimed in claim 11, wherein the monomer in step (c) is a mixture of monomers selected from methyl methacrylate (MMA) in an amount in the range of 95 to 99.5 wt. % with respect to the total weight of monomers, methacrylic acid (MAA) in an amount in the range of 0.5 to 5 wt. % with respect to the total weight of monomers, wherein the monomer in the step (e) is a mixture of monomers selected from the group consisting of methyl methacrylate (MMA) in an amount in the range of 30 to 40 wt. % with respect to the total weight of monomers, butyl methacrylate in an amount in the range of 35 to 45 wt. % with respect to the total weight of monomers, 4-hydroxy butyl acrylate in an amount in the range of 10 to 14 wt. % with respect to the total weight of monomers, methacrylamide solution in an amount in the range of 9 to 13 wt. % with respect to the total weight of monomers, methacrylic acid in an amount in the range of 0.5 to 1.5 wt. % with respect to the total weight of monomers, and 1,4-butanediol dimethacrylate (BDDMA) in an amount in the range of 1 to 3 wt. % with respect to the total weight of monomers.
18. The process as claimed in claim 11, wherein the first predetermined amount of at least one initiator is in the range of 1.5 to 3.5 wt. % with respect to the total weight of the composition and the second predetermined amount of the initiator is in the range of 1 to 3 wt. % with respect to the total weight of the composition.
19. The process as claimed in claim 11, wherein the predetermined amount of at least one buffer in the form of solution is in the range of 1.8 to 3.2 wt. % with respect to the total weight of the composition.
20. The process as claimed in claim 11, wherein the first and the second predetermined temperature is independantly in the range of 75 to 85 ºC.
21. The process as claimed in claim 11, wherein the first predeteremined time period is in the range of 10 to 20 min, the second predetermined time period is in the range of 50 to 70 min, and the third predetermined time period is in the range of 130 to 170 min.
22. A process for preparing a wax incorporated fragrance emulsion composition, said process comprising the following steps:
a) mixing a first predetermined amount of at least one emulsifier in demineralized water at a first predetermined temperature under a first predetermined stirring speed to obtain a first mixture;
b) separately preparing a pre-emulsion by
i. mixing a predetermined amount of at least one fragrance, a predetermined amount of at least one wax to obtain a blend;
ii. adding a second predetermined amount of said emulsifier, a first predetermined amount of at least one initiator, and a predetermined amount of a monomer and water to said blend at a stirring speed of 100 rpm to 500 rpm for a time period in the range of 10 to 50 min to obtain said pre-emulsion.
c) adding a first predetermined amount of said pre-emulsion obtained in step b) to said first mixture followed by adding a second predetermined amount of at least one initiator solution, and a predetermined amount of a buffer solution at a second predetermined temperature for a first predetermined time period to obtain a second mixture;
d) adding a second predetermined amount of said pre-emulsion to the second mixture at a third predetermined temperature for a second predetermined time period to obtain a third mixture; and
e) mixing a predetermined amount of a chaser catalyst to said third mixture, followed by adding a neutralizer and a preservative to obtain said wax incorporated fragrance emulsion composition.
23. The process as claimed in claim 22, wherein the first predetermined amount of at least one emulsifier is in the range of 0.1 to 0.5 wt. % with respect to the total weight of the composition and the second predetermined amount of at least one emulsifier is in the range of 3 to 6 wt. %with respect to the total weight of the composition.
24. The process as claimed in claim 22, wherein the first predetermined amount of at least one initiator is in the range of 0.05 to 0.3 wt. % with respect to the total weight of the composition and the second predetermined amount of at least one initiator is in the range of 1 to 4 wt. % with respect to the total weight of the composition.
25. The process as claimed in claim 22, wherein said monomer is a mixture of monomers selected from the group consisting of methyl methacrylate (MMA) in an amount in the range of 90 to 93 wt. % with respect to the total weight of monomers, methacrylic acid (MAA) in an amount in the range of 1 to 4 wt. % with respect to the total weight of monomers, 1,4-butanediol dimethacrylate (BDDMA) in an amount in the range of 0.5 to 1 wt. % with respect to the total weight of monomers, and methacrylamide (20 wt% aq. solution) in an amount in the range of 3 to 8 wt. % with respect to the total weight of monomers.
26. The process as claimed in claim 22, wherein the first predetermined amount of said pre-emulsion is in the range of 3 to 7 wt. % with respect to the total weight of the pre-emulsion, and the second predetermined amount of said pre-emulsion is in the range of 93 to 97 wt% with respect to the total weight of the pre-emulsion.
27. The process as claimed in claim 22, wherein the first predetermined time period is in the range of 10 to 20 min and the second predetermined time period is in the range of 230 to 250 min.
28. The process as claimed in claim 22, wherein the first predetermined stirring speed is in the range of 100 to 300 RPM.
29. The process as claimed in any of the preceding claim, wherein said at least one wax is selected from a paraffin wax and a Licocare® RBW 102 FL (renewable wax) and wherein the predetermined amount of said wax is in the range of 0.1 to 1 wt. % with respect to the total weight of the composition.
30. The process as claimed in any of the preceding claim, wherein said fragrance is Convallaria majalis (Muguet) and wherein the predetermined amount of at least one fragrance is in the range of 2 to 12 wt. % with respect to the total weight of the composition.
31. The process as claimed in any of the preceding claim, wherein said at least one emulsifier is selected from the group consisting of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), secondary alcohol ethoxylate (Tergitol 15 S 40), sodium lauryl sulfate (SLS), alkyldiphenyloxide disulfonate (Dowfax 2A1), polyoxyethylene tridecyl ether phosphate, ammonium salt (Rhodafac 610/A25), alcohol ethoxylates (ATPOL E5731/70N), and a combination thereof.
32. The process as claimed in any of the preceding claim, wherein said initiator is selected from the group consisting of potassium persulfate, ammonium persulfate, azobisisobutyronitrile (AIBN), and a combination thereof.
33. The process as claimed in any of the preceding claim, wherein said chaser catalyst is selected from tertiary butyl hydro peroxide (TBHP), sodium formaldehyde sulfoxylate (SFS), and a combination thereof and wherein the predetermined amount of chaser catalyst in the form of solution is in the range of 1 to 4 wt. % with respect to the total weight of the composition.
34. The process as claimed in any of the preceding claim, wherein said neutralizer is selected from 2-amino-2-methyl-1-propanol (Amp-95), monoethanolamine, and a combination thereof and wherein the predetermined amount of neutralizer in the form of solution is in the range of 1 to 3.5 wt. % with respect to the total weight of the composition.
35. The process as claimed in any of the preceding claim, wherein said preservative is selected from 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150), monovalent salts of chloro-methyl, methyl isothiazolinone, and a combination thereof and wherein the predetermined amount of preservative in the form of solution is in the range of 0.5 to 3 wt. % with respect to the total weight of the composition.
, Description:FIELD
The present disclosure relates to a wax incorporated fragrance emulsion composition and a process for its preparation.
DEFINITION
As used in the present disclosure, the following term is generally intended to have the meaning as set forth below, except to the extent that the context in which it is used to indicate otherwise.
Emulsion: The term “Emulsion” refers to a mixture of two or more liquids that are normally immiscible (unmixable or unblendable) owing to liquid-liquid phase separation.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Fragrances are extremely volatile material and their pleasing scent tends to weaken away very quickly. Loss of scent during manufacturing, storage, and use is very ordinary problem due to its volatile nature. Also, the fragrance material is very unstable over time. So, considering these downside, it is advantageous in the products that the fragrance is released slowly over time as the most volatile fragrances are accountable for the fresh feeling experience. Such slow release is known as extended or sustained release. Encapsulation is a way to enhance the stability of volatile and labile ingredients such as fragrances or flavors, by shielding them from all kinds of possible aggressions or degradation processes such as oxidation. Moreover, encapsulation is also a means to provide slow-release of an active ingredient, which is spread out over a more or less extended period of time, instead of trigger release. In other words, encapsulation system allows to slow down the release of active ingredients, therefore suitable for utilization in applications wherein a controlled release is required. Currently, the fragrance encapsulated systems are based on polystyrene-acrylate system and melamine formaldehyde system. However, Fragrance encapsulation by the polystyrene-acrylate system does not release the fragrance for an extended period of time. Existing melamine formaldehyde system for fragrance encapsulation does not provide shear stability of capsule. Diverse methods for encapsulation of the fragrance have been anticipated in the literature that have drawbacks such as trigger release of fragrance material, unstablility of fragrance material over time, and use of sonication and homogenization in the process. Sonication and homogenization are only practical for small scale process and this process is time-consuming as well.
There is, therefore, felt a need for a fragrance emulsion composition that can mitigate the drawbacks mentioned herein above.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
An object of the present disclosure is to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a wax incorporated fragrance emulsion composition.
Still another object of the present disclosure is to provide an effective composition which can prevent the trigger release of fragrance material and provide the better stability of fragrance material over time.
Yet another object of the present disclosure is to provide a process for the preparation of the wax incorporated fragrance emulsion composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure relates to a wax incorporated fragrance emulsion composition comprising: a wax incorporated fragrance having a ratio of wax to fragrance in the range of 1:8 to 1:40 by weight, a layer of at least one copolymer, at least one emulsifier, at least one preservative, at least one neutralizer, and q.s water.
The present disclosure further provides a process for the preparation of the wax incorporated fragrance emulsion composition. Firstly, a predetermined amount of wax and a predetermined amount of fragrance is mixed at a first predetermined temperature for a first predetermined time period to obtain a homogenous mixture. Then, a first predetermined amount of at least one emulsifier and demineralized water are added to the homogenous mixture to obtain a second mixture. Further, a predetermined amount of a first mixture of monomers is added to the second mixture to obtain a third mixture. Further, a first predetermined amount of at least one initiator and a first predetermined amount of a buffer solution are added to the third mixture at a second predetermined temperature and maintaining the second predetermined temperature for a second predetermined time period to obtain a fourth mixture. Further, a second predetermined amount of the emulsifier, a second predetermined amount of the initiator, and either a predetermined amount of a second mixture of monomers or a predetermined amount of a pre-emulsion are added to the fourth mixture for a third predetermined time period to obtain a fifth mixture. A predetermined amount of a chaser catalyst solution followed by a predetermined amount of a neutralizer and a predetermined amount of a preservative in the form of solution are added into the fifth mixture to obtain a wax incorporated fragrance emulsion composition.
Still further, the present disclosure provides a process for the preparation of the wax incorporated fragrance emulsion composition. Firstly, a first predetermined amount of at least one emulsifier is mixed in demineralized water at a first predetermined temperature under a first predetermined stirring speed to obtain a first mixture. Then, a predetermined amount of at least one fragrance, a predetermined amount of at least one wax, a second predetermined amount the emulsifier, a first predetermined amount at least one initiator, and a predetermined amount of monomer, and demineralized water are mixed separately to prepare a pre-emulsion. Further, a first predetermined amount of the pre-emulsion, a second predetermined amount of an initiator in the form of solution, and a predetermined amount of a buffer in the form of solution is added into first mixture at a second predetermined temperature for a first predetermined time period to obtain a second mixture. Further, a second predetermined amount of the pre-emulsion is added to the second mixture at a third predetermined temperature for a second predetermined time period to obtain a third mixture. A predetermined amount of a chaser catalyst in the form of solution is added into the third mixture to obtain a fourth mixture. Subsequently, a predetermined amount of a neutralizer in the form of solution and a preservative in the form of solution is added into fourth mixture to obtain a wax incorporated fragrance emulsion composition.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
The present disclosure will now be described with the help of the accompanying drawing, in which:
Figure I illustrate the fragrance release profile of the fragrance emulsion composition (A) comprising wax incorporated fragrance emulsion by using seeded emulsion polymerization and fragrance emulsion composition (B) by using seeded emulsion polymerization without using wax.
DETAILED DESCRIPTION
Embodiments, of the present disclosure, will now be described with reference to the accompanying drawing.
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open-ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
Fragrances are profoundly unstable material and its wonderful scent will in general blur away rapidly. Fragrance misfortune during assembling, stockpiling, and use is a typical downside because of its unstable nature. Likewise, the fragrance material is totally unstable after some time, bringing about loss of fragrance during capacity. Since the most volatile fragrances are responsible for the fresh feeling experience, hence, it is appealing that unstable fragrances are delivered in a controlled manner over time.
Numerous methods for encapsulation of the fragrance have been anticipated in the literature that have following drawbacks such as trigger release of fragrance material, unstable over time, and the use of sonication and homogenization in the process.
The present disclosure relates to a wax incorporated fragrance emulsion composition.
The wax incorporated fragrance emulsion composition comprises: a wax incorporated fragrance having a ratio of wax to fragrance in the range of 1:8 to 1:40 by weight; a layer of at least one copolymer; at least one emulsifier; at least one preservative, at least one neutralizer, and q.s water.
In accordance with the embodiments of the present disclosure, the wax is at least one selected from a paraffin wax and a Licocare RBW 102 FL (renewable wax). In an exemplary embodiment, the wax is paraffin wax.
In accordance with the embodiments of the present disclosure, the fragrance is Convallaria majalis (Muguet fragrance).
Convallaria majalis, commonly known as lily-of-the-valley, is a rhizomatous herbaceous perennial that typically forms an indefinitely-spreading ground cover to 8-12” tall. It is native to Europe, but has escaped cultivation and naturalized over time throughout much of temperate eastern and central North America plus parts of the Northwestern USA.
Typically, the fragrance used in the present disclosure has a floral or a fruity scent.
In accordance with the embodiments of the present disclosure, the ratio of the wax to the fragrance is in the range 1:8 to 1:40 by weight. In an exemplary embodiment, the ratio of the wax to the fragrance is 1: 20 by weight. In an another exemplary embodiment, the ratio of the wax to the fragrance is 1:8 by weight.
The fragrance and wax are mixed in such a way that fragrance dissolves completely in the wax and thus reduces the vapour pressure/volatility, and increase the effective boiling point of the fragrance.
In accordance with the embodiments of the present disclosure, the wax has high pour point in the range of 40 to 80 ºC.
In accordance with the embodiments of the present disclosure, a layer of at least one copolymer is present on the wax incorporated fragrance.
In accordance with the embodiments of the present disclosure, the copolymer is prepared by using monomer selected from methyl methacrylate (MMA), methacrylic acid (MAA), 1, 4-butanediol dimethacrylate (BDDMA), methacrylamide, and a combination thereof.
In accordance with the embodiments of the present disclosure, the amount of the methyl methacrylate (MMA) is in the range of 90 to 93 wt. % with respect to total weight of monomers, the amount of the methacrylic acid (MAA) is in the range of 1 to 4 wt. % with respect to total weight of monomers, the amount of the 1, 4-butanediol dimethacrylate (BDDMA) is in the range of 0.5 to 1 wt. % with respect to total weight of monomers, and the amount of the methacrylamide (20 wt. % aq. solution) is in the range of 3 to 8 wt. % with respect to total weight of monomers. In an exemplary embodiment the amount of the methyl methacrylate (MMA) is 91.55 wt. % with respect to total weight of monomers, the amount of the methacrylic acid (MAA) is 2.11 wt. % with respect to total weight of monomers, the amount of the 1, 4-butanediol dimethacrylate (BDDMA) is 0.70 wt. % with respect to total weight of monomers and the amount of the methacrylamide (20 wt. % aq. solution) is 5 wt. % with respect to total weight of monomers.
In an exemplary embodiment of the present disclosure, the paraffin wax and Convallaria majalis (Muguet fragrance) is coated with a layer of a copolymer prepared using methyl methacrylate (MMA) in amount of 91.55 wt. % with respect to total weight of monomers, methacrylic acid (MAA) in amount of 2.11 wt. % with respect to total weight of monomers, 1, 4-butanediol dimethacrylate (BDDMA) in amount of 0.70 wt. % with respect to total weight of monomers, and methacrylamide (20 wt. % aq. solution) in amount of 5 wt. % with respect to total weight of monomers.
In accordance with the embodiments of the present disclosure, the emulsifier is selected from the group consisting of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), secondary alcohol ethoxylate (Tergitol 15 S 40), sodium lauryl sulfate (SLS), alkyldiphenyloxide disulfonate (Dowfax 2A1), polyoxyethylene tridecyl ether phosphate, ammonium salt (Rhodafac 610/A25), alcohol ethoxylates (ATPOL E5731/70N), and a combination thereof. In an exemplary embodiment, the emulsifier is a mixture of sodium salt of fatty alcohol ether sulphate (Disponil FES 32) and secondary alcohol ethoxylate (Tergitol 15 S 40).
In accordance with the embodiments of the present disclosure, the preservative is selected from the 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150), monovalent salts of chloro-methyl, methyl isothiazolinone (Nipacide®CI 15 MV), and a combination thereof. In an exemplary embodiment, the emulsifier is 5-chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150).
In accordance with the embodiments of the present disclosure, the neutralizer is selected from 2-amino-2-methyl-1-propanol, monoethanolamine, and a combination thereof. In an exemplary embodiment, the neutralizer is 2-amino-2-methyl-1-propanol (Amp-95).
In accordance with the embodiments of the present disclosure, the composition is in the form of particles having size in the range of 100 to 300 nm. In an exemplary embodiment, the particle size is 150 nm.
In accordance with the embodiments of the present disclosure, the amount of the solid content is in the range of 40 to 50 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of the solid content is 43.5 wt. % with respect to the total weight of the composition.
The wax incorporated fragrance emulsion composition of the present disclosure, provides long lasting effect of the fragrance in a slow release manner by avoiding trigger release of fragrance over extended period of time. The wax incorporated fragrance emulsion composition of the present disclosure, has mechanical, freeze-thaw, and accelerated storage stability.
In a second aspect of the present disclosure, there is provided with a process for the preparation of the wax incorporated fragrance emulsion composition. The process is described in details as follows:
Firstly, a predetermined amount of wax and a predetermined amount of fragrance is mixed at a first predetermined temperature for a first predetermined time period to obtain a homogenous mixture.
In accordance with the embodiments of the present disclosure, the wax is at least one selected from paraffin wax and Licocare RBW 102 FL (renewable wax). In an exemplary embodiment, the wax is paraffin wax.
In accordance with the embodiments of the present disclosure, the predetermined amount of the wax is in the range of 0.1 to 1 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of wax is 0.5 wt. %.
In accordance with the embodiments of the present disclosure, the fragrance is Convallaria majalis (Muguet fragrance).
Typically, the fragrance used in the present disclosure has a floral or a fruity scent.
In accordance with the embodiments of the present disclosure, the predetermined amount of the fragrance is in the range of 2 to 5 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of fragrance is 4 wt. %.
In accordance with the embodiments of the present disclosure, the first predetermined temperature is in the range of 75 to 85 ºC. In an exemplary embodiment, the first predetermined temperature is 80 ºC.
In accordance with the embodiments of the present disclosure, the first predetermined time period is in the range of 10 to 20 min. In an exemplary embodiment, the first predetermined time period is 15 min.
In the second step, a first predetermined amount of at least one emulsifier and demineralized water are added to the homogenous mixture to obtain a second mixture.
In accordance with the embodiments of the present disclosure, the emulsifier is at least one selected from the group consisting of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), secondary alcohol ethoxylate (Tergitol 15 S 40), sodium lauryl sulfate (SLS), alkyldiphenyloxide disulfonate (Dowfax 2A1), polyoxyethylene tridecyl ether phosphate, ammonium salt (Rhodafac 610/A25), and alcohol ethoxylates (ATPOL E5731/70N). In an exemplary embodiment, the emulsifier is a mixture of sodium salt of fatty alcohol ether sulphate (Disponil FES 32) and secondary alcohol ethoxylate (Tergitol 15 S 40).
In accordance with the embodiments of the present disclosure, the first predetermined amount of at least one emulsifier is in the range of 1 to 4 wt% with respect to the total weight of the composition. In an exemplary embodiment, the first predetermined amount of at least one emulsifier is 2.3 wt. %.
In the third step, a predetermined amount of a first mixture of monomers is added to the second mixture to obtain a third mixture.
In accordance with the embodiments of the present disclosure, the first mixture of monomers is the mixture of monomers selected from methyl methacrylate (MMA) in an amount in the range of 95 to 99.5 wt. % with respect to total weight of monomers, methacrylic acid (MAA) in an amount in the range of 0.5 to 5 wt. % with respect to the total weight of monomers. In an exemplary embodiment, the amount of methyl methacrylate (MMA) is 98.76 wt.% with respect to the total weight of monomers and methacrylic acid (MAA) is 1.23 wt.% with respect to the total weight of monomers.
In the fourth step, a first predetermined amount of at least one initiator solution and a predetermined amount of a buffer solution are added to the third mixture at a second predetermined temperature and maintaining the second predetermined temperature for a second predetermined time period to obtain a fourth mixture.
In accordance with the embodiments of the present disclosure, the initiator is at least one selected from the group consisting of potassium persulfate, ammonium persulfate, and azobisisobutyronitrile (AIBN). In an exemplary embodiment, the initiator is potassium persulfate.
In accordance with the embodiments of the present disclosure, the first predetermined amount of initiator solution is in the range of 1.5 to 3.5 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 2.6 wt. %.
In accordance with the embodiments of the present disclosure, the buffer is sodium bicarbonate based buffer in the form of solution.
In accordance with the embodiments of the present disclosure, the predetermined amount of the buffer in the form of solution is in the range of 1.8 to 3.2 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of buffer solution is 2.6 wt. %.
In accordance with the embodiments of the present disclosure, the second predetermined temperature is in the range of 75 to 85 ºC. In an exemplary embodiment, the second predetermined temperature is 80 ºC.
In accordance with the embodiments of the present disclosure, the second predetermined time period is in the range of 50 to 70 min. In an exemplary embodiment, the second predetermined time period is 60 min.
In the fifth step, a second predetermined amount of the emulsifier, a second predetermined amount of the initiator, and either a predetermined amount of a second mixture of monomers or a predetermined amount of a pre-emulsion are added to the fourth mixture for a third predetermined time period to obtain a fifth mixture.
In accordance with the embodiments of the present disclosure, the second predetermined amount of the emulsifier is in the range of 1 to 3 wt % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 1.5 wt %.
In accordance with the embodiments of the present disclosure, the second predetermined amount of the initiator solution is in the range of 1 to 3 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of the initiator solution is 2.1 wt. %.
In accordance with the embodiments of the present disclosure, the second mixture of monomers is a mixture of monomers selected from the group consisting of methyl methacrylate (MMA) in an amount in the range of 30 to 40 wt. % with respect to the total weight of monomers, butyl methacrylate in an amount in the range of 35 to 45 wt. % with respect to the total weight of monomers, 4-hydroxy butyl acrylate in an amount in the range of 10 to 14 wt. % with respect to the total weight of monomers, methacrylamide solution in an amount in the range of 9 to 13 wt. % with respect to the total weight of monomers, methacrylic acid in an amount in the range of 0.5 to 1.5 wt. % with respect to the total weight of monomers, and 1,4-butanediol dimethacrylate (BDDMA) in an amount in the range of 1 to 3 wt. % with respect to the total weight of monomers. In an exemplary embodiment, the amount of methyl methacrylate (MMA) is 34.63 wt.% with respect to the total weight of monomers, the amount of butyl methacrylate is 37.51 wt.% with respect to the total weight of monomers, the amount of 4-hydroxy butyl acrylate is 12.98 wt.% with respect to the total weight of monomers, the amount of methacrylamide solution is 11.54 wt.% with respect to the total weight of monomers, the amount of methacrylic acid is 1.15 wt.% with respect to the total weight of monomers, and the amount of 1,4-butanediol dimethacrylate (BDDMA) is 2.16 wt.% with respect to the total weight of monomers.
In accordance with the embodiments of the present disclosure, the pre-emulsion is prepared by mixing a predetermined amount of at least one emulsifier, a predetermined amount of initiator, and a predetermined amount of at least one monomer.
In accordance with the embodiments of the present disclosure, the pre-emulsion comprises wax or fragrance or both. In an exemplary embodiment, the pre-emulsion comprises wax. In another exemplary embodiment, the pre-emulsion comprises at least one fragrance. In a further exemplary embodiment, the pre-emulsion comprises wax and fragrance.
In accordance with the embodiments of the present disclosure, the third predetermined time period is in the range of 100 to 200 min. In an exemplary embodiment, the third predetermined time period is 150 min.
In accordance with the embodiments of the present disclosure, the fifth step is optionally repeated up to three times to obtain the wax incorporated fragrance emulsion composition with multiple shells. In an exemplary embodiment, the fifth step is repeated up to three times to obtain the wax incorporated fragrance emulsion composition with three shells.
In the sixth step, a predetermined amount of a chaser catalyst solution followed by a predetermined amount of a neutralizer in the form of solution and a predetermined amount of a preservative in the form of solution are added into the fifth mixture to obtain the wax incorporated fragrance emulsion composition.
In accordance with the embodiments of the present disclosure, the chaser catalyst is selected from tertiary butyl hydro peroxide (TBHP), sodium formaldehyde sulfoxylate (SFS), and a combination thereof. In an exemplary embodiment, the chaser catalyst is a mixture of tertiary butyl hydro peroxide (TBHP) and sodium formaldehyde sulfoxylate (SFS).
In accordance with the embodiments of the present disclosure, the predetermined amount of the chaser catalyst in the form of solution is in the range of 1 to 4 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of the chaser catalyst solution is 2 wt. %.
In accordance with the embodiments of the present disclosure, the neutralizer is selected from 2-amino-2-methyl-1-propanol (Amp-95), monoethanolamine, and a combination thereof. In an exemplary embodiment, the neutralizer is 2-amino-2-methyl-1-propanol (Amp-95).
In accordance with the embodiments of the present disclosure, the predetermined amount of the neutralizer in the form of solution is in the range of 1.5 to 3.5 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of neutralizer solution is 2.5 wt. %.
In accordance with the embodiments of the present disclosure, the preservative is selected from 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150), monovalent salts of chloro-methyl, methyl isothiazolinone (Nipacide®CI 15 MV), and a combination thereof. In an exemplary embodiment, the preservative is 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150).
In accordance with the embodiments of the present disclosure, the predetermined amount of the preservative in the form of solution is in the range of 1.8 wt% to 2.8 wt % with respect to the total weight of the composition. In an exemplary embodiment, the amount of preservative solution is 2.2 wt. %.
In accordance with the embodiments of the present disclosure, the amount of water is in the range of 30 to 40 wt% with respect to the total weight of the composition. In an exemplary embodiment, the amount of demineralized water is 34.29 wt. %.
In third aspect of the present disclosure, there is provided a process for the preparation of the wax incorporated fragrance emulsion composition. The process is described in details as follows:
Firstly, a first predetermined amount of at least one emulsifier is mixed in demineralized water at a first predetermined temperature under a first predetermined stirring speed to obtain a first mixture.
In accordance with the embodiments of the present disclosure, the at least one emulsifier is selected from the group consisting of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), secondary alcohol ethoxylate (Tergitol 15 S 40), sodium lauryl sulfate (SLS), alkyldiphenyloxide disulfonate (Dowfax 2A1), polyoxyethylene tridecyl ether phosphate, ammonium salt (Rhodafac 610/A25), and alcohol ethoxylates (ATPOL E5731/70N). In an exemplary embodiment, the emulsifier is mixture of sodium salt of fatty alcohol ether sulphate (Disponil FES 32) and secondary alcohol ethoxylate (Tergitol 15 S 40).
In accordance with the embodiments of the present disclosure, the first predetermined amount of at least one emulsifier is in the range of 0.1 to 0.5 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 0.3 wt. %.
In accordance with the embodiments of the present disclosure, the first predetermined temperature is in the range of 75 to 85 ºC. In an exemplary embodiment, the first predetermined temperature is 80 ºC.
In accordance with the embodiments of the present disclosure, the first predetermined stirring speed is in the range of 100 to 300 RPM. In an exemplary embodiment, the first predetermined stirring speed is 200 RPM.
In the second step, separately, a predetermined amount of at least one fragrance, a predetermined amount of at least one wax, a second predetermined amount an emulsifier, a first predetermined amount of at least one initiator, and a predetermined amount of monomer, and demineralized water are mixed to prepare a pre-emulsion.
In accordance with the embodiments of the present disclosure, the pre-emulsion is prepared by:
i) A predetermined amount of at least one wax and a predetermined amount of at least one fragrance is mixed at a temperature in the range of 40 to 80 ºC under stirring to obtain a blend.
ii) Further, a second predetermined amount an emulsifier, a first predetermined amount of at least one initiator, a predetermined amount of monomer, and water is added to the blend at a stirring speed of 100 to 500 RPM for a time period in the range of 10 to 50 min to obtain the pre-emulsion.
In accordance with the embodiments of the present disclosure, the fragrance is Convallaria majalis (Muguet fragrance).
Typically, the fragrance used in the present disclosure has a floral or a fruity scent.
In accordance with the embodiments of the present disclosure, the predetermined amount of the fragrance is in the range of 6 to 12 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of fragrance is 10 wt. %.
In accordance with the embodiments of the present disclosure, the wax is at least one selected from the group consisting of paraffin wax and Licocare RBW 102 FL (renewable wax). In an exemplary embodiment, the wax is paraffin wax.
In accordance with the embodiments of the present disclosure, the predetermined amount of the wax is in the range of 0.3 to 0.75 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of wax is 0.5 wt. %.
In accordance with the embodiments of the present disclosure, the second predetermined amount of the emulsifier is in the range of 3 to 6 wt % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 4.3 wt %.In accordance with the embodiments of the present disclosure, the at least one initiator is selected from the group consisting of potassium persulfate, ammonium persulfate, and azobisisobutyronitrile (AIBN). In an exemplary embodiment, the initiator is potassium persulfate.
In accordance with the embodiments of the present disclosure, the first predetermined amount of initiator is in the range of 0.05 to 0.3 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 0.16 wt. %. In accordance with the embodiments of the present disclosure, the second predetermined amount of initiator in the form of solution is in the range of 1 to 4 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount is 1.75 wt. %.
In accordance with the embodiments of the present disclosure, the monomer is selected from the group consisting of methyl methacrylate (MMA), methacrylic acid (MAA), 1,4-butanediol dimethacrylate (BDDMA), methacrylamide), and a combination thereof. In an exemplary embodiment, the monomer is a mixture of methyl methacrylate (MMA), methacrylic acid (MAA), 1, 4-butanediol dimethacrylate (BDDMA), and methacrylamide (20 wt% aq. solution).
In accordance with the embodiments of the present disclosure, the predetermined amount of the methyl methacrylate (MMA) is in the range of 90 to 93 wt. % with respect to total weight of monomers; the predetermined amount of the methacrylic acid (MAA) is in the range of 1 to 4 wt. % with respect to total weight of monomers; the predetermined amount of the 1, 4-butanediol dimethacrylate (BDDMA) is in the range of 0.5 to 1 wt. % with respect to total weight of monomers, and the predetermined amount of the methacrylamide (20 wt% aq. solution) is in the range of 3 to 8 wt. % with respect to total weight of monomers. In an exemplary embodiment the amount of the methyl methacrylate (MMA) is 91.55 wt. % with respect to total weight of monomers, the amount of the methacrylic acid (MAA) is 2.11 wt. % with respect to total weight of monomers, the amount of the 1, 4-butanediol dimethacrylate (BDDMA) is 0.70 wt. % with respect to total weight of monomers, and the amount of the methacrylamide (20 wt. % aq. solution) is 5 wt. % with respect to total weight of monomers.
In the third step, a first predetermined amount of a pre-emulsion, a second predetermined amount of an initiator in the form of solution and a predetermined amount of a buffer in the form of solution is added to the first mixture at a second predetermined temperature for a first predetermined time period to obtain a second mixture.
In accordance with the embodiments of the present disclosure, the first predetermined amount of pre-emulsion is in the range of 3 to 7 wt. % with respect to total weight of the pre-emulsion. In an exemplary embodiment, the first predetermined amount of pre-emulsion is 5 wt. % with respect to total weight of the pre-emulsion.
In accordance with the embodiments of the present disclosure, the buffer is sodium bicarbonate based buffer in the form of solution. In accordance with the embodiments of the present disclosure, the predetermined amount of the buffer in the form of solution is in the range of 1 to 4 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of buffer is 1.75 wt. %.
In accordance with the embodiments of the present disclosure, the second predetermined temperature is in the range of 75 to 85 ºC. In an exemplary embodiment, the second predetermined temperature is 80 ºC.
In accordance with the embodiments of the present disclosure, the first predetermined time period is in the range of 10 to 20 min. In an exemplary embodiment, the first predetermined time period is 15 min.
In the fourth step, the second predetermined amount of the pre-emulsion is added to the second mixture at a third predetermined temperature for a second predetermined time period to obtain a third mixture.
In accordance with the embodiments of the present disclosure, the second predetermined amount of the pre-emulsion is in the range of 93 to 97 wt. % with respect to total weight of the pre-emulsion. In an exemplary embodiment, the first predetermined amount of pre-emulsion is 95 wt. % with respect to total weight of the pre-emulsion.
In accordance with the embodiments of the present disclosure, the third predetermined temperature is in the range of 75 to 85 ºC. In an exemplary embodiment, the third predetermined temperature is 80 ºC.
In accordance with the embodiments of the present disclosure, the second predetermined time period is in the range of 200 to 300 min. In an exemplary embodiment, the second predetermined time period is 240 min.
In the fifth step, a predetermined amount of a chaser catalyst in the form of solution is added to the third mixture to obtain a fourth mixture.
In accordance with the embodiments of the present disclosure, the chaser catalyst is selected from tertiary butyl hydro peroxide (TBHP), sodium formaldehyde sulfoxylate (SFS), and a combination thereof. In an exemplary embodiment, the chaser catalyst is a mixture of tertiary butyl hydro peroxide (TBHP) and sodium formaldehyde sulfoxylate (SFS).
In accordance with the embodiments of the present disclosure, the predetermined amount of the chaser catalyst in the form of solution is in the range of 1 to 5 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of the chaser catalyst solution is 1.78 wt. %.
In the sixth step, a predetermined amount of a neutralizer in the form of solution and a predetermined amount of preservative in the form of solution is added to the fourth mixture to obtain a wax incorporated fragrance emulsion composition.
In accordance with the embodiments of the present disclosure, the neutralizer is selected from 2-amino-2-methyl-1-propanol (Amp-95), monoethanolamine, and a combination thereof. In an exemplary embodiment, the neutralizer is 2-amino-2-methyl-1-propanol (Amp-95).
In accordance with the embodiments of the present disclosure, the predetermined amount of the neutralizer in the form of solution is in the range of 1 to 3 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of neutralizer is 1.5 wt. %.
In accordance with the embodiments of the present disclosure, the preservative is selected from the 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150), monovalent salts of chloro-methyl, methyl isothiazolinone (Nipacide®CI 15 MV), and a combination thereof. In an exemplary embodiment, the preservative is 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one mixture (Kathon LX 150).
In accordance with the embodiments of the present disclosure, the predetermined amount of the preservative in the form of solution is in the range of 0.5 to 2 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of preservative is 0.91 wt. %.
In accordance with the embodiments of the present disclosure, the amount of the water is in the range of 45 to 55 wt. % with respect to the total weight of the composition. In an exemplary embodiment, the amount of demineralized water is 49 wt. %.
In accordance with the embodiments of the present disclosure, the wax incorporated fragrance emulsion composition is filtered through a nylon mesh having size of 80.
In accordance with the embodiments of the present disclosure, the wax incorporated fragrance emulsion composition is prepared by employing the technology of seeded emulsion polymerization. The technology of seeded emulsion polymerization is advantageous in controlling the polymerization rate and the particle size of emulsion polymer at large scale.
The process for the preparation of the wax incorporated fragrance emulsion composition is simple and economical. The wax incorporated fragrance emulsion composition provides a slow release of fragrance over an extended period of time and has mechanical, freeze-thaw, and accelerated storage stability.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment but are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be tested to scale up to industrial/commercial scale and the results obtained can be extrapolated to the industrial scale.
EXPERIMENTAL DETAILS:
Experiment 1: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure (Use of mixture of monomers):
a) 5 gram of paraffin wax and 40 gram of Muguet fragrance were mixed at 80 ºC for 15 minutes to obtain a homogeneous mixture in a reactor.
b) 15 gram of secondary alcohol ethoxylate (Tergitol 15 S 40) and 8 gram of sodium salt of fatty alcohol ether sulphate (Disponil FES 32) and 240 gram of demineralized water were added to the homogenous mixture to obtain a second mixture.
c) 81 gram of a mixture of monomers (80 gram of methyl methacrylate and 1 gram of methacrylic acid) was added to the second mixture to obtain a third mixture.
d) 26 gram of potassium persulfate solution (1 gram of potassium persulfate was dissolved in 25 gram water) and 26 gram of sodium bicarbonate buffer solution (1 gram of sodium bicarbonate buffer was dissolved in 25 gram water) were added into the third mixture at 80 ºC and maintained the temperature for 60 min. to obtain a fourth mixture.
e) 10 gram of secondary alcohol ethoxylate (Tergitol 15 S 40) and 5 gram of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), 100 gram of demineralized water, 21 gram of potassium persulfate solution (1 gram of potassium persulfate was dissolved in 20 gram water) were added to the fourth mixture. 346.5 gram of a mixture of monomers (120 gram of methyl methacrylate, 130 gram of butyl methacrylate, 45 gram of 4-hydroxy butyl acrylate, 40 gram of methacrylamide (20 wt. % solution), 4 gram of methacrylic acid, and 7.5 gram of BDDMA) were added to the fourth mixture for 150 min. to obtain a fifth mixture.
f) 10.5 gram solution of tertiary butyl hydro peroxide (0.5 gram of tertiary butyl hydro peroxide was dissolved in 10 gram of water), 10.5 gram solution of sodium formaldehyde sulfoxylate (0.5 gram of sodium formaldehyde sulfoxylate was dissolved in 10 gram of water), 25 gram solution of 2-amino-2-methyl-1-propanol (Amp-95) (5 gram of 2-amino-2-methyl-1-propanol (Amp-95) was dissolved in 20 gram/ml water), and 22 gram solution of 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one (Kathon LX 150) (2 gram of 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one (Kathon LX 150 was dissolved in 20 gram of water) were added into the fifth mixture to obtain the wax incorporated fragrance emulsion composition.
Experiment 2: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure (Use of pre-emulsion instead of mixture of monomers):
Part a: Preparation of a pre-emulsion: 5 gram of paraffin wax was heated at 60 ºC for 10 minutes to liquefy in a vessel. To the above prepared liquid wax, 10 gram of secondary alcohol ethoxylate (Tergitol 15 S 40) and 5 gram of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), 105 gram of demineralized water, 21 gram of potassium persulfate (1 gram of potassium persulfate was dissolved in 20 gram water), 346.5 gram of a mixture of monomers (120 gram of methyl methacrylate, 130 gram of butyl methacrylate, 45 gram of 4-hydroxy butyl acrylate, 40 gram of methacrylamide (20 wt. % solution), 4 gram of methacrylic acid, and 7.5 gram of BDDMA) were added at a stirring speed of 300 RPM for 30 min. to obtain the pre-emulsion.
Part b: Wax incorporated fragrance emulsion composition was prepared in a manner similar to experiment 1, except 492.5 gram of the pre-emulsion as prepared in part (a) of the experiment 2 was added in the step (e) of the experiment 1 instead of 346.5 gram mixture of monomers.
Experiment 3: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure (Use of pre-emulsion comprising fragrance):
Part a: The pre-emulsion used in experiment 3 was prepared in a manner similar to part a) of experiment 2 except that (i) 60 gram of fragrance was added in the pre-emulsion, (ii) no wax added in the pre-emulsion and (iii) the pre-emulsion was not heated.
Part b: The experiment 3 was performed in a similar manner as detailed in part b) of experiment 2, except that pre-emulsion as prepared in step (a) of Experiment 3 was used instead of the pre-emulsion as prepared in Experiment 2, part a).
Experiment 4: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure (Use of pre-emulsion comprising wax and fragrance):
The experiment 4 was performed in a similar manner as detailed in part b) of experiment 2, except 246.2 gram of the pre-emulsion as prepared in the part b) of the experiment 2 and 246.2 gram of the pre-emulsion as prepared in the part a) of the experiment 3 were used instead of the pre-emulsion as prepared in Experiment 2, part a).
Experiment 5: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure (preparation of multiple (3) shells):
The experiment 5 was performed in a similar manner as detailed in experiment 1, except the step (e) in experiment 1 was repeated 3 times before the step (f) to obtain the wax incorporated fragrance emulsion having 3 shells.
Experiment 6: Preparation of wax incorporated fragrance emulsion composition in accordance with the present disclosure
2.1 gram of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), 1.5 gram of secondary alcohol ethoxylate (Tergitol 15 S 40), and 200 gram of demineralized water were added at 80 ºC at a stirring speed of 200 RPM to obtain a first mixture.
Separately, 5 gram of paraffin wax, 100 gram of Muguet fragrance was mixed with each other at 60 ºC to obtain a blend. To the above prepared blend of wax and fragrance 22 gram of secondary alcohol ethoxylate (Tergitol 15 S 40), 195 gram of demineralized water, 30 gram of sodium salt of fatty alcohol ether sulphate (Disponil FES 32), 2 gram of potassium persulfate, 355 gram of a mixture of monomers (325 gram of methyl methacrylate, 20 gram of methacrylamide(20 wt. % solution), 7.5 gram of methacrylic acid, and 2.5 gram of BDDMA), and 195 gram of demineralized water were added at a stirring speed of 300 RPM for 30 min to obtain the pre-emulsion.
34.95 gram of the so obtained pre-emulsion, 21 gram solution of potassium persulfate (1 gram of potassium persulfate was dissolved in 20 gram water), 21 gram of solution sodium bicarbonate based buffer (1 gram of sodium bicarbonate based buffer was dissolved in 20 gram water), were added into the first mixture at a temperature of 80 ºC for 15 min to obtain a second mixture.
674.05 gram of remaining pre-emulsion was added to the second mixture at 80 ºC for 240 min to obtain a third mixture.
10.7 gram solution of tertiary butyl hydro peroxide (0.7 gram of tertiary butyl hydro peroxide was dissolved in 10 gram of water), 10.7 gram solution of sodium formaldehyde sulfoxylate (0.7 gram of sodium formaldehyde sulfoxylate was dissolved in 10 gram of water), 18 gram solution of 2-amino-2-methyl-1-propanol (Amp-95) (5 gram of 2-amino-2-methyl-1-propanol (Amp-95) was dissolved in 13 gram water), and 11 gram solution of 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one (Kathon LX 150) (2 gram of 5-Chloro-2-methyl-4-isothiazolin-3-one-2-methyl-4-isothiazolin-3-one (Kathon LX 150) was dissolved in 9 gram of water) was added into the fourth mixture to obtain the wax incorporated fragrance emulsion composition.
The composition was exposed at 120 ºC for 1 hr (the water completely evaporates at 120ºC for 1 hr) and after that solid content was calculated and it was found to be 43.5%. The particle size of the so obtained composition is 150 nm.
Experiment 7 was carried in a similar manner as mentioned in experiment 1 without use of wax.
Experiment 8: Fragrance Release profile study
Measurement of fragrance release profile:
The wax encapsulated fragrance emulsion composition of the present disclosure (A) and the fragrance encapsulated emulsion composition without wax (B) were taken to study the fragrance release profile.
To generate the release profile, the weight loss for the compositions A and B were calculated at 45ºC.
1g of wax encapsulated fragrance emulsion composition of sample (A) was taken in the lid appropriately and weight loss was measured at various interval of time. Further, 1g of fragrance encapsulated emulsion composition without wax of sample (B) was taken in the lid appropriately and weight loss was measured at various interval of time. The graph was plotted between the percent weight loss and the time interval at constant temperature (45ºC).
It is evident from the Fig. I that 50% fragrance release has been restricted in fragrance incorporated emulsion using wax (A) compared to fragrance incorporated emulsion without wax (B).
TECHNICAL ADVANCEMENTS
The present disclosure described hereinabove has several technical advantages including, but not limited to, the realization of a wax incorporated fragrance emulsion composition that:
• provides a slow release of fragrance over extended period of time;
• avoids trigger release of fragrance;
• have long lasting effect of fragrance; and
• has mechanical, freeze-thaw, and accelerated storage stability.
The embodiments herein and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the embodiments herein.
The foregoing description of the specific embodiments so fully reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the disclosure to achieve one or more of the desired objects or results.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values mentioned for the various physical parameters, dimensions or quantities are only approximations and it is envisaged that the values higher/lower than the numerical values assigned to the parameters, dimensions or quantities fall within the scope of the disclosure, unless there is a statement in the specification specific to the contrary.
While considerable emphasis has been placed herein on the components and component parts of the preferred embodiments, it will be appreciated that many embodiments can be made and that many changes can be made in the preferred embodiments without departing from the principles of the disclosure. These and other changes in the preferred embodiment as well as other embodiments of the disclosure 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 disclosure and not as a limitation.
| # | Name | Date |
|---|---|---|
| 1 | 202121010097-STATEMENT OF UNDERTAKING (FORM 3) [10-03-2021(online)].pdf | 2021-03-10 |
| 2 | 202121010097-REQUEST FOR EXAMINATION (FORM-18) [10-03-2021(online)].pdf | 2021-03-10 |
| 3 | 202121010097-PROOF OF RIGHT [10-03-2021(online)].pdf | 2021-03-10 |
| 4 | 202121010097-POWER OF AUTHORITY [10-03-2021(online)].pdf | 2021-03-10 |
| 5 | 202121010097-FORM 18 [10-03-2021(online)].pdf | 2021-03-10 |
| 6 | 202121010097-FORM 1 [10-03-2021(online)].pdf | 2021-03-10 |
| 7 | 202121010097-FIGURE OF ABSTRACT [10-03-2021(online)].jpg | 2021-03-10 |
| 8 | 202121010097-DRAWINGS [10-03-2021(online)].pdf | 2021-03-10 |
| 9 | 202121010097-DECLARATION OF INVENTORSHIP (FORM 5) [10-03-2021(online)].pdf | 2021-03-10 |
| 10 | 202121010097-COMPLETE SPECIFICATION [10-03-2021(online)].pdf | 2021-03-10 |
| 11 | Abstract1.jpg | 2021-10-19 |
| 12 | 202121010097-FER.pdf | 2022-12-28 |
| 13 | 202121010097-FORM 3 [12-01-2023(online)].pdf | 2023-01-12 |
| 14 | 202121010097-OTHERS [28-06-2023(online)].pdf | 2023-06-28 |
| 15 | 202121010097-MARKED COPIES OF AMENDEMENTS [28-06-2023(online)].pdf | 2023-06-28 |
| 16 | 202121010097-FORM 13 [28-06-2023(online)].pdf | 2023-06-28 |
| 17 | 202121010097-FER_SER_REPLY [28-06-2023(online)].pdf | 2023-06-28 |
| 18 | 202121010097-DRAWING [28-06-2023(online)].pdf | 2023-06-28 |
| 19 | 202121010097-COMPLETE SPECIFICATION [28-06-2023(online)].pdf | 2023-06-28 |
| 20 | 202121010097-CLAIMS [28-06-2023(online)].pdf | 2023-06-28 |
| 21 | 202121010097-AMMENDED DOCUMENTS [28-06-2023(online)].pdf | 2023-06-28 |
| 22 | 202121010097-PatentCertificate28-02-2024.pdf | 2024-02-28 |
| 23 | 202121010097-IntimationOfGrant28-02-2024.pdf | 2024-02-28 |
| 1 | muguetE_22-12-2022.pdf |