CN105419945B - Essence microcapsule and preparation method thereof - Google Patents
Essence microcapsule and preparation method thereof Download PDFInfo
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- CN105419945B CN105419945B CN201511007644.4A CN201511007644A CN105419945B CN 105419945 B CN105419945 B CN 105419945B CN 201511007644 A CN201511007644 A CN 201511007644A CN 105419945 B CN105419945 B CN 105419945B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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Abstract
The invention provides an essence microcapsule and a preparation method thereof. The essence microcapsule has a core-shell structure, and comprises: a capsule core; and a capsule wall wrapping the capsule core. The capsule core is made of essence; the capsule wall is melamine formaldehyde resin filled with inorganic nano particles and modified by polyvinyl alcohol. The essence microcapsule of the invention has low release rate, good heat resistance, strong oxidation resistance, long service life and low toxicity.
Description
Technical Field
The invention relates to the field of essence, in particular to an essence microcapsule and a preparation method thereof.
Background
The essence and the spice are products closely related to human life and are widely applied to various fields. The essence is mostly used in a low amount in various products, but plays a very important role in the quality of the products, and is called as the soul of the perfumed products. However, the essence has many problems in the using process, for example, as a volatile product, the essence is easily volatilized in a large amount in the transportation, storage and use processes and is wasted, and even the product is deteriorated. The microcapsule technology can well solve the problem, and the essence is wrapped by the microcapsule to effectively reduce the volatilization of the essence during the non-use period and avoid the conflict between the essence and other substances in the product.
The existing microcapsule technology is mostly used for medicines, and the wall materials of the microcapsules have certain defects, the inoxidizability of the wall materials is weak, the coating rate of essence is low, and the utilization rate of the essence cannot be improved to a great extent.
Disclosure of Invention
In view of the problems in the background art, the invention aims to provide the essence microcapsule and the preparation method thereof, wherein the essence microcapsule has the advantages of low release rate, good heat resistance, strong oxidation resistance, long service life and low toxicity.
To achieve the above object, in one aspect of the present invention, there is provided a perfume microcapsule having a core-shell structure, comprising: a capsule core; and a capsule wall wrapping the capsule core. The capsule core is made of essence; the capsule wall is melamine formaldehyde resin filled with inorganic nano particles and modified by polyvinyl alcohol.
In another aspect of the present invention, the present invention provides a method for preparing a perfume microcapsule, comprising the steps of: (1) mixing and stirring the capsule core, an emulsifier and deionized water uniformly to obtain an emulsified capsule core, wherein the capsule core is made of essence; (2) stirring formaldehyde and melamine under a heating condition for reaction, then adding inorganic nanoparticles and polyvinyl alcohol, and continuously stirring for carrying out polymerization reaction to obtain a prepolymer of a capsule wall, wherein the capsule wall is melamine formaldehyde resin filled with the inorganic nanoparticles and modified by the polyvinyl alcohol; (3) and adding the prepolymer of the capsule wall into the emulsified capsule core, adjusting the pH value to acidity for reaction, and then stirring, filtering, and drying to finish the preparation of the essence microcapsule.
Compared with the prior art, the invention has the beneficial effects that:
the essence microcapsule has good embedding effect and high embedding rate, and effectively avoids the problem that the fragrance is dispersed during the transportation, storage and use processes of the essence.
The essence microcapsule of the invention has low release rate, good heat resistance, strong oxidation resistance, long service life and low toxicity.
The essence microcapsule of the invention can reduce the use of formaldehyde, and the polyvinyl alcohol can also react with excessive formaldehyde, thereby reducing the content of free formaldehyde in reaction liquid, improving the safety performance of the essence microcapsule and reducing the hidden danger to human health.
The essence microcapsule can be widely applied to various aspects such as vehicle-mounted essence, home decoration and the like, and has very high application prospect and practical benefit.
Drawings
Fig. 1 is an optical microscope photograph of the perfume microcapsule prepared in example 1;
FIG. 2 is a scanning electron micrograph of the perfume microcapsule prepared in example 1;
FIG. 3 is a scanning electron micrograph of a damaged perfume microcapsule prepared in example 1;
FIG. 4 is a graph showing the release rate profiles of the perfume microcapsules prepared in examples 1 and 5 to 6 and comparative examples 1 to 3.
Detailed Description
The perfume micro-capsule according to the present invention and the preparation method thereof are explained in detail below.
First, a perfume microcapsule according to a first aspect of the present invention is explained, the perfume microcapsule having a core-shell structure comprising: a capsule core; and a capsule wall wrapping the capsule core. The capsule core is made of essence. The capsule wall is melamine formaldehyde resin filled with inorganic nano particles and modified by polyvinyl alcohol.
In the essence microcapsule according to the first aspect of the present invention, the toughness and oxidation resistance of the melamine formaldehyde resin can be improved by modifying the melamine formaldehyde resin with polyvinyl alcohol. The melamine formaldehyde resin is modified mainly by introducing polyvinyl alcohol macromolecules to react to generate an acetalation product in the hydroxymethylation stage, so that the aggregation of triazine ring structures in molecules can be blocked, and the effect of enhancing the toughness of the melamine formaldehyde resin can be achieved. And the polyvinyl alcohol has certain elasticity, so that when the polyvinyl alcohol is embedded into macromolecules of the melamine formaldehyde resin, the flexibility of molecular chains of the melamine formaldehyde resin can be improved. In addition, the polyvinyl alcohol can also react with excessive formaldehyde, so that the content of free formaldehyde in the reaction liquid is reduced. The inorganic nano particles are added into the polyvinyl alcohol modified melamine formaldehyde resin as a filling material, so that the tensile strength of the polyvinyl alcohol modified melamine formaldehyde resin can be improved, the reason is that the inorganic nano particles and the polyvinyl alcohol modified melamine formaldehyde resin are physically or chemically combined, the interface bonding is enhanced, and the inorganic nano particles can bear a certain load, so that the tensile strength of the formed capsule wall is increased, the pore diameter of the capsule wall is reduced, the toughness of the capsule wall is enhanced, the release rate of the capsule core material is further slowed down, and the service life of the essence microcapsule is prolonged.
In the perfume microcapsule according to the first aspect of the present invention, the polyvinyl alcohol may have an average degree of polymerization of 1750.
In the perfume microcapsule according to the first aspect of the present invention, the ratio of the amount of formaldehyde to melamine (i.e., melamine) in the melamine formaldehyde resin may be 1:1 to 1: 1.5. The formaldehyde is a volatile organic matter, and if the content of the formaldehyde is too high, the toxicity of the essence microcapsule is too high, which is not beneficial to human health and does not meet the requirement of green chemistry.
In the essence microcapsule according to the first aspect of the present invention, the mass of the polyvinyl alcohol may be 0.5% to 0.9% of the total mass of the capsule wall.
In the flavour microcapsule according to the first aspect of the present invention, the inorganic nanoparticles may be selected from TiO2、SiO2One or two of。
In the perfume microcapsule according to the first aspect of the present invention, the mass of the inorganic nanoparticles may be 0.3% to 0.5% of the total mass of the capsule wall.
In the perfume microcapsule according to the first aspect of the present invention, the diameter (i.e., particle diameter) of the inorganic nanoparticles may be 5 to 20 nm.
In the essence microcapsule according to the first aspect of the present invention, the mass ratio of the essence to the capsule wall may be 1:1 to 2: 1.
In the essence microcapsule according to the first aspect of the present invention, the essence may be a naturally extracted essence oil or an artificially synthesized essence, and the essence oil may be one or more selected from natural rose essence oil, orange flower essence oil, sweet osmanthus flower essence oil, clove essence oil, gardenia flower essence oil, jasmine flower essence oil, lemon essence oil, bulgarian rose essence oil, lavender essence oil, and sweet almond essence oil.
In the essence microcapsule according to the first aspect of the present invention, the essential oil is selected from jasmine essential oil and sweet almond essential oil, and the mass ratio of the two may be 1: 1; or the essential oil is selected from lavender essential oil and sweet almond essential oil, and the mass ratio of the lavender essential oil to the sweet almond essential oil can be 1: 0.9; or the essential oil is selected from the rose essential oil and the orange flower essential oil, and the mass ratio of the rose essential oil to the orange flower essential oil can be 1: 1.2; or the essential oil is selected from lemon essential oil, clove essential oil, bulgaria rose essential oil and lavender essential oil, and the mass ratio of the four is 2:1:2: 1.
In the perfume microcapsule according to the first aspect of the present invention, the diameter of the perfume microcapsule may be 2 to 4 μm.
Next, a method for preparing the perfume microcapsule according to the second aspect of the present invention is described, for preparing the perfume microcapsule according to the first aspect of the present invention, comprising the steps of: (1) mixing and stirring the capsule core, an emulsifier and deionized water uniformly to obtain an emulsified capsule core, wherein the capsule core is made of essence; (2) stirring formaldehyde and melamine under a heating condition for reaction, then adding inorganic nanoparticles and polyvinyl alcohol, and continuously stirring for carrying out polymerization reaction to obtain a prepolymer of a capsule wall, wherein the capsule wall is melamine formaldehyde resin filled with the inorganic nanoparticles and modified by the polyvinyl alcohol; (3) and adding the prepolymer of the capsule wall into the emulsified capsule core, adjusting the pH value to acidity for reaction, and then stirring, filtering, and drying to finish the preparation of the essence microcapsule.
In the preparation method of the essence microcapsule according to the second aspect of the present invention, in the step (1), the emulsifier may be one or more selected from Sodium Dodecyl Sulfate (SDS), sodium dodecyl sulfate, and sodium dodecyl benzene sulfonate.
In the preparation method of the essence microcapsule according to the second aspect of the present invention, in step (1), the mass of the emulsifier may be 0.15% to 0.2% of the mass of the capsule core.
In the preparation method of the perfume microcapsule according to the second aspect of the present invention, in the step (2), the heating temperature may be 70 ℃.
In the preparation method of the essence microcapsule according to the second aspect of the present invention, in the step (3), the pH value may be adjusted to 3-4 using glacial acetic acid for reaction.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
3.0883g of melamine, 1.8364g of formaldehyde aqueous solution (mass fraction of 36 percent) and 30ml of deionized water are weighed, stirred for 40min under the condition of a constant temperature oil bath at 70 ℃, and then 0.0168g of nano TiO is added2Particles (the particle diameter is 5 nm-20 nm) and polyvinyl alcohol (PVA) aqueous solution, wherein the PVA content is 0.0312g, then stirring is carried out for 30min under the constant temperature oil bath at 70 ℃ to obtain the aqueous solution of the melamine formaldehyde resin prepolymer which is filled with the inorganic nano particles and is modified by the PVA.
4.7034g of neroli essential oil, 0.0079g of emulsifier SDS and 30ml of deionized water are weighed and stirred vigorously (the rotating speed is 1440r/min) for 60min to obtain the emulsified capsule core.
Adding an aqueous solution of a melamine formaldehyde resin prepolymer which is filled with inorganic nanoparticles and modified by polyvinyl alcohol into an emulsified capsule core, adding 3-4 drops of n-amyl alcohol to eliminate foam, adjusting the pH to 3.0 by using glacial acetic acid, then violently stirring (the rotating speed is 1440r/min) for 60min at 70 ℃, carrying out suction filtration after the reaction is finished, washing for 2-3 times by using absolute ethyl alcohol, and naturally airing to obtain the essence microcapsule.
Example 2
Weighing 3.0129g of melamine, 1.8567g of formaldehyde aqueous solution (mass fraction of 36%) and 30ml of deionized water, stirring for 40min under a constant-temperature oil bath at 70 ℃, and then adding 0.0172g of nano TiO2Particles (the particle diameter is 5 nm-20 nm) and polyvinyl alcohol (PVA) aqueous solution, wherein the PVA content is 0.0310g, then stirring is carried out for 30min under the constant temperature oil bath at 70 ℃ to obtain the aqueous solution of the melamine formaldehyde resin prepolymer which is filled with the inorganic nano particles and is modified by the PVA.
Weighing 4.2g of osmanthus essential oil, 0.0082g of emulsifier SDS and 30ml of deionized water, and violently stirring (the rotating speed is 1440r/min) for 60min to obtain the emulsified capsule core.
Adding an aqueous solution of a melamine formaldehyde resin prepolymer which is filled with inorganic nanoparticles and modified by polyvinyl alcohol into an emulsified capsule core, adding 3-4 drops of n-amyl alcohol to eliminate foam, adjusting the pH to 3.0 by using glacial acetic acid, then violently stirring (the rotating speed is 1440r/min) for 60min at 70 ℃, carrying out suction filtration after the reaction is finished, washing for 2-3 times by using absolute ethyl alcohol, and naturally airing to obtain the essence microcapsule.
Example 3
3.1012g of melamine, 1.9937g of formaldehyde aqueous solution (mass fraction of 36 percent) and 30ml of deionized water are weighed, stirred for 40min under the condition of a constant temperature oil bath at 70 ℃, and then 0.0115g of nano TiO is added2Particles (the particle diameter is 5 nm-20 nm) and polyvinyl alcohol (PVA) aqueous solution, wherein the PVA content is 0.0314g, then the reaction is continued under oil bath with constant temperature of 70 ℃ for 30min, and the aqueous solution of melamine formaldehyde resin prepolymer which is filled with inorganic nano particles and is modified by the PVA is obtained.
4.7743g of lemon essential oil, 0.0084g of emulsifier SDS and 30ml of deionized water are weighed and stirred vigorously (the rotating speed is 1440r/min) for 60min to obtain the emulsified capsule core.
Adding an aqueous solution of a melamine formaldehyde resin prepolymer which is filled with inorganic nanoparticles and modified by polyvinyl alcohol into an emulsified capsule core, adding 3-4 drops of n-amyl alcohol to eliminate foam, adjusting the pH to 3.0 by using glacial acetic acid, then violently stirring (the rotating speed is 1440r/min) for 60min at 70 ℃, carrying out suction filtration after the reaction is finished, washing for 2-3 times by using absolute ethyl alcohol, and naturally airing to obtain the essence microcapsule.
Example 4
3.0304g of melamine, 1.4612g of formaldehyde aqueous solution (mass fraction of 36 percent) and 30ml of deionized water are weighed, stirred for 40min under the condition of a constant temperature oil bath at 70 ℃, and then 0.0174g of nano TiO is added2Particles (the particle diameter is 5 nm-20 nm) and polyvinyl alcohol (PVA) aqueous solution, wherein the PVA content is 0.0314g, then stirring is carried out for 30min under the constant temperature oil bath at 70 ℃ to obtain the aqueous solution of the melamine formaldehyde resin prepolymer which is filled with the inorganic nano particles and is modified by the PVA.
3.5664g of lemon essential oil, 0.0059g of emulsifier SDS and 30ml of deionized water are weighed and stirred vigorously (the rotating speed is 1440r/min) for 60min to obtain the emulsified capsule core.
Adding an aqueous solution of a melamine formaldehyde resin prepolymer which is filled with inorganic nanoparticles and modified by polyvinyl alcohol into an emulsified capsule core, adding 3-4 drops of n-amyl alcohol to eliminate foam, adjusting the pH to 3.0 by using glacial acetic acid, then violently stirring (the rotating speed is 1440r/min) for 60min at 70 ℃, carrying out suction filtration after the reaction is finished, washing for 2-3 times by using absolute ethyl alcohol, and naturally airing to obtain the essence microcapsule.
Example 5
Perfume microcapsules are prepared according to the method of example 1, except that nano TiO2The mass of the particles was 0.0115 g.
Example 6
Perfume microcapsules are prepared according to the method of example 1, except that nano TiO2The mass of the particles was 0.019 g.
Comparative example 1
Perfume microcapsules were prepared according to the method of example 1, except that no nano TiO was added2Particles and PVA.
Comparative example 2
Perfume microcapsules were prepared according to the method of example 1, except that no nano TiO was added2Particles, only PVA was added.
Comparative example 3
Perfume microcapsules were prepared according to the method of example 1, except that no PVA was added, only nano TiO was added2Particles.
The perfume microcapsules are then characterized for the relevant properties.
(1) Dispersing the prepared essence microcapsules by using a small amount of ethyl acetate, preparing an optical microscope sample, and observing and photographing.
(2) And taking a picture of the prepared essence microcapsule by using a scanning electron microscope.
(3) And drying the prepared essence microcapsules, and then putting the dried essence microcapsules into a weighing bottle for periodic weighing to obtain a release curve.
Referring to fig. 1, an optical microscope photograph of the perfume microcapsule prepared in example 1 shows that the perfume microcapsule prepared in the present invention is spherical. Referring to fig. 2 and fig. 3, scanning electron micrographs of the essence microcapsules prepared in example 1 and damaged essence microcapsules show that the surface of the essence microcapsules prepared in the present invention is not smooth and has punctate protrusions, and the punctate protrusions are formed by the action of inorganic nanoparticles and PVA-modified melamine formaldehyde resin.
Referring to fig. 4, which is a release curve of the essence microcapsules prepared in examples 1 and 5-6 and comparative examples 1-3, the ordinate represents the quality of the essence microcapsules, and it can be seen from fig. 4 that the release rate of the essence microcapsules of the present invention is greatly reduced, and the sealing effect is better.
The sealing performance of the perfume microcapsules prepared in comparative example 1 was the worst, and the sealing performance of the perfume microcapsules prepared in comparative examples 2 to 3, although slightly improved, was still unsatisfactory. The reason is that the mechanical properties of pure PVA modified melamine formaldehyde resin or inorganic nanoparticle filled melamine formaldehyde resin are poor, so that the mechanical properties of the capsule wall of the essence microcapsule are poor.
As can be seen from the comparison between example 1 and comparative examples 1 to 3, the sealing performance of the perfume microcapsule is obviously improved by using the melamine formaldehyde resin which is filled with the inorganic nanoparticles and is modified by the polyvinyl alcohol in example 1. The melamine formaldehyde resin filled with the inorganic nanoparticles and modified by the polyvinyl alcohol has better coating effect on the essence, and the obtained essence microcapsule has adjustable particle size, narrow particle size distribution (the diameter is about 2-4 μm, and the diameter is combined with the figure 2 and the figure 3), and high coating rate (99%).
From the comparison between example 1 and examples 5 to 6, it is found that the optimum amount of the inorganic nanoparticles to be added to the capsule wall is present.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A perfume microcapsule, the perfume microcapsule having a core-shell structure comprising:
a capsule core; and
a capsule wall wrapping the capsule core;
it is characterized in that the preparation method is characterized in that,
the capsule core is made of essence;
the capsule wall is melamine formaldehyde resin filled with inorganic nano particles and modified by polyvinyl alcohol;
wherein the content of the first and second substances,
the mass ratio of formaldehyde to melamine is 1:1 to 1: 1.5;
the mass of the polyvinyl alcohol is 0.5-0.9% of the total mass of the capsule wall;
the mass of the inorganic nano particles is 0.3-0.5% of the total mass of the capsule wall.
2. A perfume microcapsule according to claim 1, wherein the inorganic nanoparticles are selected from TiO2、SiO2One or two of them.
3. The flavor microcapsule according to claim 1 or 2, wherein the inorganic nanoparticles have a diameter of 5nm to 20 nm.
4. The essence microcapsule according to claim 1, wherein the mass ratio of the essence to the capsule wall is 1: 1-2: 1.
5. The essence microcapsule according to claim 1, wherein the essence is a naturally extracted essence oil or an artificially synthesized essence, and the essence oil is one or more selected from orange flower essence oil, sweet osmanthus flower essence oil, clove essence oil, gardenia essence oil, jasmine essence oil, lemon essence oil, bulgaria rose essence oil, lavender essence oil and sweet almond essence oil.
6. The flavor microcapsule of claim 1, wherein the flavor microcapsule has a diameter of 2 μm to 4 μm.
7. A process for the preparation of a perfume microcapsule according to any of claims 1 to 6, comprising the steps of:
(1) mixing and stirring the capsule core, an emulsifier and deionized water uniformly to obtain an emulsified capsule core, wherein the capsule core is made of essence;
(2) stirring formaldehyde and melamine under a heating condition for reaction, then adding inorganic nanoparticles and polyvinyl alcohol, and continuously stirring for carrying out polymerization reaction to obtain a prepolymer of a capsule wall, wherein the capsule wall is melamine formaldehyde resin filled with the inorganic nanoparticles and modified by the polyvinyl alcohol;
(3) and adding the prepolymer of the capsule wall into the emulsified capsule core, adjusting the pH value to acidity for reaction, and then stirring, filtering, and drying to finish the preparation of the essence microcapsule.
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| CN106397675B (en) * | 2016-06-23 | 2019-02-01 | 华南师范大学 | A kind of preparation method of core-shell type nano essence capsule |
| CN106433976A (en) * | 2016-12-16 | 2017-02-22 | 东莞波顿香料有限公司 | Slow release microencapsulated flavor and preparation method thereof |
| CN106955652A (en) * | 2017-04-11 | 2017-07-18 | 广州秘理普植物技术开发有限公司 | A kind of essence microcapsule and preparation method thereof |
| CN107455492A (en) * | 2017-08-07 | 2017-12-12 | 西南林业大学 | A kind of method that nano-silicon dioxide modified microcapsule wall material prepares microcapsules |
| CN107969730B (en) * | 2017-11-23 | 2020-04-14 | 北京亚美方舟科贸有限公司 | Preparation method of tobacco flavor microcapsule |
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| CN109464319A (en) * | 2018-11-02 | 2019-03-15 | 东莞波顿香料有限公司 | Breath freshening capsule and preparation method thereof |
| CN109705994B (en) * | 2018-12-25 | 2021-03-16 | 广东爱车小屋电子商务科技有限公司 | Decontamination flavor enhancer and preparation method thereof |
| CN111534285A (en) * | 2020-06-01 | 2020-08-14 | 长沙理工大学 | SiO (silicon dioxide)2Preparation method of modified phase-change microcapsule |
| CN113999726B (en) * | 2021-08-18 | 2023-09-15 | 江苏集萃先进高分子材料研究所有限公司 | Essential oil microcapsule and preparation method thereof |
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| CN102059083A (en) * | 2010-11-26 | 2011-05-18 | 北京化工大学 | Method for preparing phase-transformation microcapsule with wall material inlaid with nano alumina |
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| CN103464068A (en) * | 2013-09-06 | 2013-12-25 | 上海应用技术学院 | Pressure-sensitive melamine resin essence microcapsule and preparation method thereof |
| CN103641366B (en) * | 2013-11-25 | 2016-04-13 | 深圳大学 | The preparation method of epoxy microcapsule |
| CN103709445B (en) * | 2013-12-30 | 2016-01-06 | 云南省化工研究院 | A kind of preparation method of the melmac coated ammonium polyphosphate had excellent water-resistance |
| BR102014008536A2 (en) * | 2014-04-09 | 2015-12-01 | Vollmens Fragrances Ltda | polymeric microcapsule for extended release of assets and their manufacturing process |
| CN104230608B (en) * | 2014-08-14 | 2016-07-06 | 中国工程物理研究院化工材料研究所 | Melamine resin in-situ polymerization prepares the method for high explosive microcapsule |
| CN104888671B (en) * | 2015-05-05 | 2017-07-04 | 南雄市星隆化工有限公司 | A kind of double shell microcapsule and preparation method and application |
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