Abstract: The present invention describes an encapsulated system comprising (a) an inner oil phase comprising fragrances (oils) and flavors; and (b) an outer matrix phase comprising at least three polymers, multivalent metal ions, wherein the polymer: oil ratio ranges from 1:1 to 19:1. The fragrances are retained by the microcapsules for a long period of time. The present invention also provided a process for the preparation of the microcapsules along with the ink formulations.
CLIAMS:1. An encapsulated system comprising
a. an inner oil phase comprising fragrances (oils) and flavors; and
b. an outer matrix phase comprising at least three polymers, multivalent metal ions
Wherein the polymer: oil ratio ranges from 1:1 to 19:1
2. The encapsulated system as claimed in claim 1 wherein said oil phase comprises of essential oil, other oils, oils-soluble ingredients and their mixtures.
3. The encapsulated system as claimed in claim 1 wherein said matrix phase comprises of polymers and their mixtures.
4. The encapsulated system as claimed in claim 1 wherein said encapsulatyed system has a particle size ranging from 0.1 to 10 µm, preferably from 0.2 to 6 µm and more preferably from 0.2 to 4 µm.
5. The encapsulated system as claimed in claim 1 wherein said polymers are selected from the group consisting of Acacia, PVAc, Sodium alginate, xanthan, carrageenan, CMC, Tamarind gum, Gum Karaya, Dextran, Gelatin, Gluten, Gaur gum, Pectin and the like.
6. The encapsulated system as claimed in claim 5 wherein said sodium alginate ranges from 1 to 10 % w/w.
7. The encapsulated system as claimed in claim 5 wherein said polymers ranges from 0.5 to 15% w/w.
8. The encapsulated system as claimed in claim 1 wherein said multivalent metal ions are selected from the group consisting of calcium chloride, ferric chloride and mixture thereof.
9. The encapsulated system as claimed in claim 1 wherein ranges amount of said multivalent metal ion from 1-10% w/w.
10. The encapsulated system as claimed in claim 1 wherein said fragrances are selected from group consisting of essential oils, carrier oils, synthetic fragrance oils, oil soluble synthetic chemicals (fragrance/flavor) and mixture thereof.
11. The encapsulated system as claimed in claim 1 wherein said fragrance ranges from 0.5 to 20% w/w., preferably from 08 to 15% w/w.
12. A process for the preparation of an encapsulated system comprising steps of
a) mixing polymers and water to make a solution and homogenizing the same
b) adding fragrances to the homogenized mixture of step (a);
c) adding multivalent metal ions and water to make a solution; and
d) obtaining the microcapsules.
13. A process for the preparation of an ink formulation comprising steps of
a. weighing sodium alginate and gum acacia;
b. adding water to make solution;
c. adding fragrance and homogenizing;
d. adding weighed quantity of Poly vinyl Acetate and homogenizing;
e. adding measured quantity of 5% Calcium Chloride solution and homogenizing;
f. adding more quantity of Polyvinyl Acetate;
g. adding weighed quantity of Red Phosphorus and mixing; and
h. applying this ink on the specified portion of match box surface with the help of brush or an inkjet printer ,TagSPECI:Field of the invention
The present invention relates to uniform microcapsules comprising of fragrance and/or flavor that is compatible with ink formulation which is printed on the side surface of the match box. The fragrances are retained by the microcapsules for a long period of time.
Background of the invention
Safety matches are considered ‘safe’ because they don't spontaneously combust. In order to get the match stick ignited, one would have to strike them against a special surface or striking surface provided on the match box. The match heads contain sulfur sometimes antimony III sulfide) and oxidizing agents (usually potassium chlorate), with powdered glass, colorants, fillers, and a binder made of glue and starch. The striking surface consists of powdered glass or silica (sand), red phosphorus, binder, and filler. When the safety match is struck, the glass-on-glass friction generates heat, converting a small amount of red phosphorus to white phosphorus vapor. White phosphorus spontaneously ignites, decomposing potassium chlorate and liberating oxygen. At this point, the sulfur starts to burn, which ignites the wood of the match.
Match boxes conventionally has a coarse striking surface on one edge for lighting the matches contained inside. The match stick head has fire-starting chemical which when rubbed with the side of match produces fire. The side surface of matchstick has ink printed on it. The fire starting chemicals in general consists of phosphorous and sulphur which are associated with bad odor/foul smell upon ignition, which is generally non-acceptable among people having allergy. It is therefore desirable to eliminate or mask the level of foul smell associated with the use of matchstick.
US8119175 relates to matrix particles encapsulating flavors and fragrances in a discontinuous phase of inclusions of oil dispersed within in a continuous phase of polymeric matrix material. The oil may be used as a carrier for the active, or may be an active in its own right. This invention provides a means for protecting sensitive actives from harsh environments, and for releasing such materials in a time-dependent fashion. This prior art further discloses a method SD2, in which the spray-dried particles are hardened by cross-linking alginate and the said particles are introduced to a solution of multivalent cations, e.g. ions of calcium, strontium, barium, iron, silver, aluminum, manganese, copper and zinc, preferably calcium in the form of calcium chloride solution, preferably of 0.9-2%. US’175 relate to incorporation of fragrance or flavors into the matrix system wherein the fragrance are held inside the polymer matrix. The object of prior art is to make hard solid particles by spray drying the emulsion and adding it to calcium chloride solution.
US20060246265 relates to a substrate that is generally flat material and capable of being scented by applying a scented material to the substrate by one or more of the following ways: including scented material into the substrate, applying scented material to one or more surfaces of the substrate, and/or including scented material in a coating, such as a wax, plastic or rubber coating, applied to the substrate. The invention discloses that scented material may be intermittently and/or strategically applied to the substrate and the scented material is any material suitable for imparting a scent to the particular substrate utilized and may be a microencapsulated formulation (such as a scented ink or scratch and sniff material) applied to one or more surfaces of the substrate and/or a material that is included in the substrate, such as an essential oil. It is further disclosed that the scented material may be applied during a printing process. The microcapsules releases scent/perfume upon rupturing by pressure or heat as applied by a user, such as by touching, rubbing or scratching the microcapsules, or by the application of water, a chemical or some other stimulus. US’265 teach products wherein the fragrances or flavor referred as scented materials are fixed using wax like materials. The invention disclosed in US ’265 describes the use of microcapsules prepared as per the prior art to be used as a scented material for surface printing.
US5093182 relates to a sustained-release perfume-containing coating obtained from a non-aqueous solution or dispersion of a selected polymeric material such as ethyl cellulose in perfume oil for application to a substrate of an advertising sampler or the like in combination with an ink-printed image applied to the same article. Coatings described in this prior art may be readily applied to a variety of substrates and in particular to paper sheets or cards suitable for use as advertising samplers. The coatings may be applied by various means, and they are suitable for being supplied on a large scale process by conventional printing equipment. US ‘182 also provides a sustained-release, perfume-containing coating that may be applied to paper or other substrates having printed images thereon without producing a reaction between perfume oils and the ink present in such images. It is further disclosed that premature loss of more volatile, top-note components of the fragrance, which would result in a degraded rendition of the fragrance blend, is prevented; and the possibility of adulteration of the fragrance by reaction with other components such as waxes, solvents, plasticizers, or an aqueous phase that have been used in prior coated compositions may be avoided by including only the polymer and perfume oil. US ’182 relate to incorporation of fragrance or flavors into the polymer system. Formulation is just an admixture of polymer and fragrances.
WO2007036814 relates to a cigarette that contains a flavorant encapsulated with polyvinyl acetate, where heat and/or moisture are used to release the flavorant from the polyvinyl acetate encapsulation into mainstream of smoke during smoking. WO ‘814 discloses a filtered cigarette comprising of a substantially cylindrical tobacco rod, cylindrical filter rod and a tipping paper circumscribing and joining the filter rod and the tobacco rod wherein the filter rod includes a flavorant encapsulated by polyvinyl acetate. This invention provides a method of flavoring mainstream tobacco smoke, comprising: retaining a flavorant (menthol) with a polyvinyl acetate matrix and releasing menthol from the matrix while generating mainstream smoke, said releasing step includes an application of heat and/or moisture to the matrix. WO ’814 relate to cigarette that contains a flavorant encapsulated with polyvinyl acetate. Encapsulates in prior art are prepared by spraying alcohol polymer and fragrance mixture over the surface to form small globules.
Prior art reported many attempts to solve the problem by designing a fragrance containing match stick which when ignited releases the fragrance inside it. One attempt to solve the said problem is to incorporate fragrance in the ink formulation which is used to print the side surface of the matchstick box. Fragrances and flavors are volatile in nature and it is a challenge to make them compatible and stable within the ink formulation. However none of the methods described so far dealt with formation of fragrance encapsulated microcapsules that are compatible with the ink formulation printed on the striking surface of match box such that fragrance is released when the user strikes the match stick on the striking surface of match box.
The present invention therefore identifies the need to develop a consumer friendly approach to solve the present problem by providing fragrance encapsulated microcapsules that are not only compatible with the ink formulation printed on the striking surface of match box but also remain fragrant for longer periods.
Objects of invention
An object of the present invention is to overcome the drawbacks of the prior art.
Another object of the present invention to provide a consumer friendly approach to mask or to eliminate the level of foul smell associated with the use of match stick.
Yet another object of the present invention is to provide an ink formulation comprising of fragrance encapsulated microcapsules that can be printed on the striking surface of match box.
Yet another object of the present invention is to ensure that the unique combination of fragrance microcapsules remain stable in the ink formulation painted over the striking surface of match box for longer periods.
Summary of the present invention
An aspect of the present invention is to provide an encapsulated system comprising
a. an inner oil phase comprising fragrances (oils) and flavors; and
b. an outer matrix phase comprising at least 3 polymers, multivalent metal ions
wherein the polymer: oil ratio ranges from 1:1 to 19:1
Another aspect of the present invention is to provide a process for the preparation of an encapsulated system comprising steps of
Step 1: mixing polymers and water to make a solution and homogenizing the same
Step 2: adding fragrances to the homogenized mixture of step (a);
Step 3: adding multivalent metal ions and water to make a solution; and
Step 4: obtaining the microcapsules.
Yet another aspect of the present invention is to provide a process for the preparation of an ink formulation comprising steps of
Step 1: weighing sodium alginate and gum acacia;
Step 2: adding water to make solution;
Step 3: adding fragrance and homogenizing;
Step 4: adding weighed quantity of Poly vinyl Acetate and homogenizing;
Step 5: adding measured quantity of 5% Calcium Chloride solution and homogenizing;
Step 6: adding more quantity of Polyvinyl Acetate;
Step 7: adding weighed quantity of Red Phosphorus and mixing; and
Step 8: applying this ink on the specified portion of match box surface with the help of brush or an inkjet printer
Brief Description of the Accompanying Drawings
Figure 1 illustrates microcapsules of the present invention prepared according to the process described in Example-1.
Figure 2 illustrates microcapsules of the present invention prepared according to the process described in Example-2.
Figure 3 illustrates microcapsules prepared according to the process described in non-working example (Example-3).
Figure 4 illustrates the formation of fragrance microcapsules initially when prepared at (t0).
Figure 5 illustrates the microscopic view of fragrance microcapsules stored for 60 days at 50C (10X40).
Figure 6 illustrates the microscopic view of fragrance microcapsules stored for 60 days at 25 0C (10X40).
Figure 7 illustrates the microscopic view of fragrance microcapsules stored for 60 days at 40 0C Rh 75% (10X40).
Figure 8 illustrates microscopic view of microcapsule of the present invention and the same of the prior art.
Detailed Description of the Invention
Match boxes conventionally has a coarse striking surface on one edge for lighting the matches contained inside. The match stick head has fire-starting chemical which when rubbed with the side of match produces fire. The side surface of match box has ink printed on it. The invention provides in-situ formation of microcapsules suitable for striking surface which is formed automatically during formulating the ink. The present method can also be very conveniently adapted to the existing scale up process of production of matchsticks by just incorporation of homogenizer.
In accordance with the present invention an encapsulated system is provided comprising two distinct phases having oil phase and matrix phase wherein the oil phase is separated from matrix phase by a physical boundary of polymer matrix wall.
The term “encapsulated system” as used herein includes fragrance or flavor globule encapsulated in capsule having a polymer composite wall.
The term “microcapsules” as used herein refers to fragrance globule encapsulated into a composite wall that is made of polymer matrix.
Oil phase is composed of essential oil, oil, oil-soluble ingredients and mixture thereof.
The oil may be selected from a group comprising vegetable oil, silicon oil, synthetic oil, mono, di and tri glycerides and the like.
Matrix phase is composed of polymers and mixture thereof.
In one of the embodiments of present invention, uniform fragrance microcapsules having particle size of 0.25-4 micron is provided comprising of fragrance and/or flavor that is compatible with ink formulation which is printed on the side surface of the match box. The particle size of the microcapsules disclosed in the present invention varies from 0.1 to 10 µm, preferably from 0.2 to 6 µm and more preferably from 0.2 to 4 µm. The said microcapsule is incorporated suitably in the ink formulation that is printed on the striking surface of the matchstick box. The unique composition of the fragrance microcapsules ensures that these remain stable in the ink formulation. It is also noted that match box coated with ink comprising fragrance microcapsules of the present invention remain fragrant for over and above 2 months as compared to matchboxes without the said microcapsules which remain fragrant only for a week.
In a preferred composition, the said microcapsules comprise of composite wall, composed of polymers and multivalent metal ions and fragrances and flavors entrapped in it. The microcapsules of the invention are formed out of particular polymer compositions and comprise unique polymer: oil ratio. The total polymer to oil ratio varies from 1:1 to 19:1.
As oil is insoluble in the matrix medium it can be expected that all oil are in the core. In certain case processing conditions may lead to loss of certain volatile oils.
Suitable polymers used are selected from the group consisting of Acacia, PVAc, Sodium alginate, xanthan, carrageenan, CMC, Tamarind gum, Gum Karaya, Dextran, Gelatin, Gluten, Gaur gum, and other synthetic polymers, Pectin and alike, most preferably acacia gum alginates, poly vinyl acetate.
The polymer comprises of Alginates from 1 to 10 (% w/w),
Presences of alginates are essential however other polymers can be selected from the list provided above. The polymers or are used in the range from 0.5 to 15 % w/w.
Suitable multivalent metal ions of the present invention are selected from the group consisting of calcium chloride, ferric chloride, aluminum chloride and mixture thereof. The multivalent metal ion can be used in the range from 1-10% w/w.
Suitable fragrances of present invention are selected from group consisting of essential oils, carrier oils, Synthetic fragrance oils, oil soluble synthetic chemicals (fragrance/flavor) and mixture thereof.
Suitable essential oils used in case of present invention are selected from the list of neroli oil, camphor oil, cardamom oil, carrot seed oil, juniper oil, lime oil, mandarin oil, orange oil, neem oil, peppermint oil, clary sage oil, lavender oil, jasmine oil, sandalwood oil, patchouli oil, rose mary oil, frank incense oil, wintergreen oil, green tea absolute oil, fennel oil, rose wood oil, bergamot oil, basil oil, grapefruit oil, geranium oil, lemongrass oil, cinnamon oil, ylang ylang oil, cedarwood oil, citronella oil, clove oil, eucalyptus oil, tea tree oil, almond sweet oil, avocado oil, lemon oil, linseed oil / flax seed oil, cinnamon leaf oil, clove leaf oil, orange sweet oil, olive oil, chamomile oil, (nilgiri oil), rosemary oil, rose oil, ginger oil, grape fruit oil, vetiver oil, grape seed oil, winter green oil (gaultheria oil), jojoba oil, wheat germ oil, angelica oil, balsam fir (idaho) oil, black pepper oil, blue cypress oil, blue tansy oil, celery seed oil, cinnamon bark oil, cistus oil, copaiba oil, coriander oil, cypress oil, dill oil, dorado azul oil, elemi oil, eucalyptus blue oil, eucalyptus globulus oil, eucalyptus radiata oil, frankincense oil, galbanum oil, german chamomile oil, goldenrod oil, helichrysum oil, hinoki oil, hong kuai oil, hyssop oil, idaho blue spruce, idaho tansy oil, laurus nobilis oil, ledum oil, lemon myrtle oil, marjoram oil, melaleuca (alternifolia) oil, melaleuca (ericifolia) oil, melaleuca quinquenervia oil, melissa oil, mountain savory oil, myrrh oil, myrtle oil, nutmeg oil, ocotea oil,, oregano oil, palmarosa oil, palo santo oil, peppermint oil, petitgrain oil, pine oil, ravintsara oil, roman chamomile oil, sacred frankincense oil, sage oil, spearmint oil, spikenard oil, tangerine oil, tarragon oil, thyme oil, valerian oil, xiang mao oil, musk oil, civet, castreum, ambergris, bergamot oil, sage oil, verbena oil, citronea oil, cauout oil, salvia oil, clove oil, chamomie oil, ostus oil, labdanum oil, broom oil, carrot seed oil, minmosa oil, narcissus oil, obanum oil and mixture thereof.
Suitable carrier oils used in case of present invention are selected from the list of almond oil, aloevera oil, apricot oil, calendula oil, walnut oil, sunflower oil, silicone oils, rice bran oil, soyabeen oils, almond oil, aloe vera oil, apricot kernel oil, calendula oil, evening primrose oil, hazelnut oil, macadamia oil, rosehip oil, sesame oil, walnut oil and mixture thereof.
Suitable Synthetic fragrance oils used in case of present invention are selected from the list of apple cider oil, apple maple oil, apple oil, bamboo & green tea oil, banana oil , banana nut bread oil, berry blaster oil, black cherry oil, blackberry oil, blueberry oil, bonsai tree oil, brambleberry ivy oil, buttered rum cannabis bloom oil ,caramel oil, caramel vanilla oil, cedar & balsam oil, chai latte oil, chamomile oil, chardonnay oil, bamboo jasmine oil, banana oil, cucumber oil, berry oil, black cherry oil, blackberry oil, blueberry oil, vanilla oil, cedar & balsam oil, chai latte oil, chamomile oil, tea oil, coffee oil, chardonnay oil, dragon's blood oil, eucalyptus lavender oil, frankincense & myrrh oil, French vanilla oil, fruits oil, ginger oil, gingko biloba oil, gingko ginseng oil, grapefruit mint oil, green apple oil, green tea & ginger oil, green tea oil, ,hazelnut oil, hazelnut coffee oil, hibiscus & white amber oil, lilac oil, lilac blossoms oil, lily of the valley oil, lime oil, mango oil, maple syrup oil, merlot oil, pomegranate oil, mint oil, mossberry oil, mulberry oil, nutcracker oil, nutmeg oil, oat milk & honey oil, oatmeal oil, orange vanilla oil, papaya oil, peach oil, pear oil, pearberry oil, pina colada oil, pineapple oil, plumeria oil, pomegranate oil, pumpkin oil, pumpkin thyme oil, raspberry oil, raspberry lime oil, red apple peel oil, red poppies oil, sage oil, sandalwood & amber oil, spearmint oil, spice oils, strawberry oil, sweet coconut oil, sweet pea oil, sweet woods oil, tangerine oil, tobacco blend oil, vanilla oil, vanilla coffee oil, watermelon oils and mixture thereof.
Suitable oil soluble synthetic chemicals (fragrance/flavor) used in case of present invention are selected from the list of acetophenonene, dimethindene derivatives, naphthalene derivatives, α-amylcinnamic aldehyde, anethole, anisaldehyde, benzyl acetate, benzyl alcohol, benzyl propionate, borneol, cinnamyl acetate, cinnamyl alcohol, citral citronellal, cumin aldehyde, cyclamen aldehyde, decanol, ethyl butyrate, ethyl caprate, ethyl cinnamate, ethyl vanillin, eugenol, geraniol, hexenol, α-hexylcinnamic aldehyde, hydroxycitronellal, indole, iso-amyl acetate, iso-amyl iso-valerate, iso-eugenol, linalyl acetate, p-methylacetophenone, methyl anthranilate, Methyl dihydrojasmonate, methyl eugenol, methyl β-naphthyl ketone, methylphenhlcarbinyl acetate, musk ketol, musk xylol, 2,5,6-nanodinol, γ-nanolactone, Phenylacetic aldehyde dimethyl acetal, β-phenylethyl alcohol, 3,3,5-trimethylcyclohexanol, γ- undecalactone, undecenal, vanillin, menthol, camphor and mixtures thereof and mixture thereof.
The required amount of fragrance ranges from 0.5 to 20% w/w., preferably from 8 to 15% w/w.
Another embodiment of the present invention provides a process for the preparation of microcapsules and the said process comprises of following steps:
Step 1: Mixing polymers and water to make a solution and homogenizing the same
Step 2: Adding fragrances to the homogenized mixture of step (a);
Step 3: Adding multivalent metal ions and water to make a solution; and
Step 4: Obtaining the microcapsules.
The formation of microcapsules was confirmed from microscopic observation using any bright field microscope.
The match box coated with ink comprising fragrance microcapsules of the present invention remain fragrant for over and above 3 months as compared to match boxes without the said microcapsules which remain fragrant only for a week.
Figure 5, 6 and 7 shows the microcapsules of the present invention. The figures show that the microcapsules are uniformly distributed and intact.
Microcapsules of the present invention can be prepared and stored for longer periods and then can be added with the ready ink as and when required. The samples can be prepared and stored for 60 days at different temperature conditions 50°C, 250°C and at 400°C (75% RH). It was observed that the encapsulated solution remains similar to the initial solution even after 60 days of storage at different temperature conditions. Figures 5, 6 and 7 depicts that all capsules are intact and retain same form as initial capsules prepared at t0.
In another embodiment of present invention, a single step process for the production of ink formulation is provided comprising the steps of preparing in situ formation of microcapsules of fragrances which is compatible with the striking surface of ink formulation of the matchstick.
The conventional process for the preparation of ink formulation:
Step 1: Take weighed quantity of sodium alginate and gum acacia
Step 2: Add Water to make solution
Step 3: Add Fragrance and homogenize
Step 4: Take 5% aqueous solution of Calcium chloride in a tray
Step 5: Spray the sodium alginate and Fragrance mixture in to the prepared calcium chloride solution and keep it for 10 minutes
Step 6: Centrifuge the solution to obtain microcapsules
Step 7: Take weighed quantity of phosphorus red
Step 8: Add Poly Vinyl Acetate to it
Step 9: Add required quantity of prepared microcapsules and mix it properly
Step 10: Apply this ink on the specified portion of match box surface with the help of brush
It can also be applied through inkjet printer
Observation: Ink is not uniform; hence print on the surface is not smooth. Capsules are bigger (10 times)
Process as per the present invention
Step 1: Take weighed quantity of sodium alginate and gum acacia
Step 2: Add water to make solution
Step 3: Add fragrance and homogenize
Step 4: Add weighed quantity of Poly vinyl Acetate again homogenize
Step 5: Add measured quantity of 5% Calcium Chloride solution and homogenize
Step 6: Add more quantity of Polyvinyl Acetate
Step 7: Add weighed quantity of Red Phosphorus and mix well
Step 8: Apply this ink on the specified portion of match box surface with the help of brush
It can also be applied through inkjet printer
The sequence of addition of the ingredients is very much essential for in-situ generation of the microcapsules. The process of preparation of microcapsules is merged with the process of preparing the ink in such a way that the microcapsules are formed in-situ.
Polyvinyl acetate added in step (d) is critical for the formation of microcapsules while the polyvinyl acetate added in step (f) is critical for the formation of the ink holding the microcapsules uniformly. The amount of PVA added in the step (d) is a part of ink formulation.
Observation: Ink is uniform, hence print on the surface is smooth and excellent microcapsule formation is achieved.
The process as per the present invention is advantageous over the prior art in terms of being simplified, provide uniform microcapsules which provide smooth surface finish, provide microcapsules with much smaller size that can retain fragrance for a longer period of time and microcapsules are stable for along period of time.
The expression “in-situ” as used herein refers to converting the microcapsule system into ink formulation.
Yet another embodiment of the present invention provides a process of in-situ formation of microcapsules and coating of the ink formulation on the surface of match box comprises of following steps.
Step 1: Desired quantity of sodium alginate and gum acacia is weighed
Step 2: Water is added to it to make solution
Step 3: fragrance is added and homogenized
Step 4: weighed quantity of Poly vinyl Acetate is added again and the mixture is homogenized
Step 5: Measured quantity of 5% Calcium Chloride solution is added to mixture above and homogenized
Step 6: more quantity of Polyvinyl Acetate is added and mixed properly
Step 7: weighed quantity of Red Phosphorus is added to the above mixture and mixed well to get the ink formulation
Step 8: The resulted ink is applied on the specified portion of match box surface with the help of brush or through an inkjet printer.
The present invention is now illustrated by way of non-limiting examples.
Example-1: Working Example
Table 1
Ingredients Amount (gm) % w/w
Sodium alginate 20 5.12
Acacia 10 2.56
PVAc 30 7.69
Fragrance 50 12.82
5% CaCl2 100 25.64
Water 180 46.15
Process:
Step 1: weigh Sodium alginate and acacia in a beaker, add water to make solution, keep on stirring till homogenized mixture is obtained
Step 2: Weigh fragrance and keep separate
Step 3: Weigh PVAc solution and keep separate
Step 4: weigh Calcium Chloride and add water to make 5% solution
Step 5: Add weighed fragrance to sodium alginate and acacia mixture, stir till homogenizes
Step 6: Add weighed PVAC solution and continue stirring
Step 7: Add 5% Calcium chloride solution to the above mixture and continue stirring for 10 min.
Observation: stable microcapsules formed
Example-2: working example
Table 2
Ingredients Amount (gm) % w/w
Sodium alginate 25 8.33
Acacia 10 3.33
PVAc 5 1.66
Fragrance 10 3.33
5% CaCl2 (in water) 125 41.66
Water 125 41.66
Process:
Step 1: weigh sodium alginate and acacia in a beaker, add water to make solution, keep on stirring till homogenized mixture is obtained
Step 2: Weigh fragrance and keep separate
Step 3: Weigh PVAc solution and keep separate
Step 4: weigh Calcium Chloride and add water to make 5% solution
Step 5: Add weighed fragrance to sodium alginate and acacia mixture, stir till homogenizes
Step 6: Add weighed PVAC solution and continue stirring
Step 7: Add of 5% Calcium chloride solution to the above mixture and continue stirring for 10 min.
Observation: stable microcapsules formed.
Example-3: Non-Working Example
Table 3
Ingredients Amount (gm) % w/w
Sodium alginate 15 4.87
Acacia 10 3.25
PVAc 2.5 0.81
Fragrance 5 1.62
5% CaCl2 (in water) 75 24.39
Water 200 65.04
Step 1: weigh sodium alginate and acacia in a beaker, add water to make solution, keep on stirring till homogenized mixture is obtained
Step 2: Weigh fragrance and keep separate
Step 3: Weigh PVAc solution and keep separate
Step 4: weigh Calcium Chloride and add water to make 5% solution
Step 5: Add weighed fragrance to sodium alginate and acacia mixture, stir till homogenizes
Step 6: Add weighed PVAC solution and continue stirring
Step 7: Add of 5% Calcium chloride solution to the above mixture and continue stirring for 10 min.
Observation: stable microcapsules are not formed
Example 4: Non-Working Example
Table 4
Ingredients Amount (gm) % w/w
Sodium alginate 10 4.54
Acacia 1 0.45
PVAc 7 3.18
Fragrance 2 0.90
5% CaCl2 (in water) 50 22.72
Water 150 68.18
Observation: stable microcapsules are not formed
Step 1: weigh sodium alginate and acacia in a beaker, add water to make solution, keep on stirring till homogenized mixture is obtained
Step 2: Weigh fragrance and keep separate
Step 3: Weigh PVAc solution and keep separate
Step 4: weigh Calcium Chloride and add water to make 5% solution
Step 5: Add weighed fragrance to sodium alginate and acacia mixture, stir till homogenizes
Step 6: Add weighed PVAC solution and continue stirring
Step 7: Add of 5% Calcium chloride solution to the above mixture and continue stirring for 10 min.
Example 5: Data demonstrating the working of the present invention with respect to combination of polymer and fragrance in a ratio of 1:1 to 19:1
Table 5
Ratio of polymer : oil 1:1 19:1 25:1 1:2 1:5
Ingredients % w/w % w/w % w/w % w/w % w/w
Sodium alginate 1.6 8 2.4 1 1
Acacia 0.80 4 0.24 1 2
PVAc 1.6 3 2.4 1 1
Fragrance 4 0.8 0.2 6 16
5% CaCl2 (in water) 50 50 50 50 50
Water Qs to 100 Qs to 100 Qs to 100 Qs to 100 Qs to 100
Observation A free flowing solution form having uniform distribution of microcapsule A free flowing viscous system having uniform microcapsule distribution Very thick mas Free flowing liquid that phase separates on standing Free flowing liquid that phase separates on standing
Example 6: data illustrating achieving of the desired property with the help of the microcapsule of the present invention in comparison to the composition of the prior art as also illustrated in the figures.
Table 6
S No Microcapsule of the present invention Microcapsule of the prior art
Ingredients % w/w Ingredients % w/w
1 Sodium alginate 5.12 Sodium alginate 2.5
2 Acacia 2.56 Acacia gum 1
3 PVAc 7.69 Modified starch 1
4 Fragrance 12.82 Pullulan 0.5
5 5% CaCl2 (in water) 25.64 Fragrance 10
6 Water 46.15 Water 85
2% calcium chloride solution (2gm of calcium chloride dissolved in 100 gm of water) qs
Observation Stable microcapsules formed as shown in figure 8 Microcapsules size are not uniform, capsules were big and without any oil core as shown in figure 8
Example 7 comparison of the process of preparation of the microcapsule of the prior art along with the process of the present invention
Process of preparing microcapsules of the present invention:
Step 1: weigh sodium alginate and acacia in a beaker, add water to make solution, keep on stirring till homogenized mixture is obtained
Step 2: Weigh fragrance and keep separate
Step 3: Weigh PVAc solution and keep separate
Step 4: weigh Calcium Chloride and add water to make 5% solution
Step 5: Add weighed fragrance to sodium alginate and acacia mixture, stir till homogenizes
Step 6: Add weighed PVAC solution and continue stirring
Step 7: Add 5% Calcium chloride solution to the above mixture and continue stirring for 10 min.
Observation: Stable microcapsules formed as shown in figure 8
Process of preparing microcapsules of the prior art
Step 1: Sodium alginate, acacia gum, modified starch, pullulan and fragrance are mixed with water to make slurry, and is keep on stirring under 1050 to 2000 rpm till slurry is obtained.
Step 2: weigh 2 gm Calcium Chloride and add 100 gm of water to make 2% solution
Step 3: slurry obtained from step 1 is taken into a liquid sprayer and sprayed on 2% Calcium Chloride solution obtained in step 2 in order to obtain the microcapsules.
Observation: Microcapsules size are not uniform in size, capsules were big (20 times) and without any oil core as shown in figure 8
Example 8: Stability data of the microcapsule formulation with respect to time and temperature.
Table 7
Storage time At time t0 Room temperature (25 0C) for 60 days At low temperature (50C) for 60 days At elevated temperature (40 0C and Rh 75%) for 60 days
Observation Microcapsules are found to be stable as shown in figure 9 Microcapsules are found to be stable as shown in figure 9 Microcapsules are found to be stable as shown in figure 9 Microcapsules are found to be stable as shown in figure 9
| # | Name | Date |
|---|---|---|
| 1 | GPA of ITC limited.pdf | 2014-02-25 |
| 2 | FORM 3.pdf | 2014-02-25 |
| 3 | Form 2 with complete specification as filed.pdf | 2014-02-25 |
| 4 | Drawings as filed.pdf | 2014-02-25 |
| 5 | 222-KOL-2014-(26-03-2014)-FORM-1.pdf | 2014-03-26 |
| 6 | 222-KOL-2014-(26-03-2014)-CORRESPONDENCE.pdf | 2014-03-26 |
| 7 | 222-KOL-2014-FER.pdf | 2017-11-24 |
| 8 | 222-KOL-2014-OTHERS [18-05-2018(online)].pdf | 2018-05-18 |
| 9 | 222-KOL-2014-FER_SER_REPLY [18-05-2018(online)].pdf | 2018-05-18 |
| 10 | 222-KOL-2014-PatentCertificate10-05-2019.pdf | 2019-05-10 |
| 11 | 222-KOL-2014-IntimationOfGrant10-05-2019.pdf | 2019-05-10 |
| 12 | 222-KOL-2014-RELEVANT DOCUMENTS [25-03-2020(online)].pdf | 2020-03-25 |
| 1 | TACD1_17-11-2017.pdf |