CN110711544A - Preparation method of self-adhesive aromatic microcapsule - Google Patents
Preparation method of self-adhesive aromatic microcapsule Download PDFInfo
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- CN110711544A CN110711544A CN201910967182.2A CN201910967182A CN110711544A CN 110711544 A CN110711544 A CN 110711544A CN 201910967182 A CN201910967182 A CN 201910967182A CN 110711544 A CN110711544 A CN 110711544A
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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
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
Abstract
The invention discloses a preparation method of a self-adhesive aromatic microcapsule, which comprises the following steps: (1) using essence, organic monomer, emulsifier, oily initiator and deionized water as raw materials, and preparing aromatic seed microspheres of polymer coated essence by an emulsion polymerization method; (2) the self-adhesive aromatic microcapsule is prepared by taking polymethyl methacrylate aromatic seed microspheres, dopamine, trihydroxymethyl aminomethane and deionized water as raw materials. The aromatic microcapsule taking polydopamine as the shell is prepared by a simple and controllable two-step polymerization method, the used materials meet the requirement of environmental protection, the obtained microcapsule has long fragrance retention time and good adhesion on a base material, and has potential application value in the fields of textiles, clothing, decoration, buildings and the like.
Description
Technical Field
The invention belongs to the technical field of microcapsules, and particularly relates to a preparation method of a self-adhesive aromatic microcapsule.
Background
The moderate fragrance can make people feel refreshing, and has various health-care effects of deodorizing, eliminating fatigue, relieving tension, sterilizing, tranquilizing and the like. Products with aromatic odours have become more and more popular in our lives, especially in the european and african markets, where they are in high popularity. The method for treating the needed articles by directly soaking, spraying or sprinkling substances with aromatic odor has the advantages of simplicity, convenience and quickness, is popular with consumers, and is used by common toilet water, perfume, mosquito repellent lotion and the like.
The persistence of the fragrance is one of the product points of interest to consumers. In recent years, in order to obtain fragrance products with long lasting fragrance, researchers have developed various methods in which substances having a fragrant odor are microencapsulated in the simplest and most effective manner. The microencapsulated fragrant product is called fragrant microcapsule, and as the fragrant substance is coated in the shell layer of the microcapsule, the shell layer can obstruct the transmission of the fragrant smell to a certain extent, so the fragrant microcapsule has the advantage of prolonging the fragrance-retaining time of the fragrant substance, and has wider application in the fields of cosmetics, clothes and decorative lamps. However, current fragrance microcapsule products also have significant disadvantages in that, after they are applied to a substrate by post-treatment means such as dipping, spraying, and showering, since they are generally bonded to the substrate by physical action such as van der waals force, hydrogen bonding, and the like, the microcapsules are easily detached from the substrate after being subjected to friction, water washing, and the like, resulting in a decrease in fragrance function of the substrate. For the base materials which are required to be subjected to long perfume-retaining time and friction, water washing and the like, the development of the perfume microcapsule which is long in perfume-retaining time and strong in adhesion has a more prominent practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of a self-adhesive aromatic microcapsule, wherein dopamine is an endogenous nitrogen-containing organic compound, and a polymer polydopamine of the dopamine has the performance similar to that of mussel adhesive protein and shows good adhesion. Based on the experience of long-term working on the preparation and application of the aromatic microcapsule, the invention provides the preparation of the aromatic microcapsule with polydopamine as an outer shell layer, and aims to obtain a microcapsule product with long fragrance retention time and strong adhesion. The microcapsule has double shell layers and good self-adhesion, is beneficial to enriching the types of aromatic microcapsule products and promoting the development and application of aromatic functional products.
In order to solve the technical problems, the following technical scheme is adopted:
a preparation method of self-adhesive aromatic microcapsules is characterized by comprising the following steps:
(1) the aromatic seed microspheres of polymer-coated essence are prepared by taking essence, organic monomers, an emulsifier, an oily initiator and deionized water as raw materials through an emulsion polymerization method, wherein the polymerization temperature is 75 ℃, and the reaction time is 10h
(2) The preparation method comprises the steps of preparing the self-adhesive aromatic microcapsule by taking aromatic seed microspheres of essence coated by a polymer, dopamine, trihydroxymethyl aminomethane and deionized water as raw materials, wherein the polymerization reaction temperature is 30 ℃, and the reaction time is 24 hours.
Preferably, in the step (1), the mass of the organic monomer is 5 times of that of the essence, the mass ratio of the essence to the deionized water is 1:20, the emulsifier accounts for 3% of the mass of the essence, and the oily initiator accounts for 2% of the mass of the organic monomer.
Preferably, the essence in the step (1) is rose, lavender, jasmine and cologne-fragrance essence.
The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the organic monomer in the step (1) is one of methyl methacrylate and styrene.
Preferably, the emulsifier in step (1) is one of cetyltrimethyl ammonium bromide, cetyltrimethyl ammonium chloride and lauryl sodium sulfate.
Preferably, the oily initiator in the step (1) is one of azobisisobutyronitrile and benzoyl peroxide.
Preferably, the aromatic seed microspheres in the step (2) account for 10% of the mass of the deionized water, the dopamine accounts for 2% of the mass of the deionized water, and the tris (hydroxymethyl) aminomethane accounts for 1% of the mass of the deionized water.
Preferably, the pH value of the reaction liquid obtained after the raw materials are mixed in the step (2) is 8.5.
Due to the adoption of the technical scheme, the method has the following beneficial effects:
the invention relates to a preparation method of self-adhesive aromatic microcapsules, which is characterized in that aromatic microcapsules taking polydopamine as shells are prepared by a simple and controllable two-step polymerization method, the used materials meet the requirements of environmental protection, the obtained microcapsules have long fragrance retention time and good adhesion on a base material, and have potential application values in the fields of textiles, clothes, decoration, buildings and the like.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a scanning electron microscope photograph of the aromatic microcapsules of example 1 of the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying examples, in order to fully understand the objects, features and effects of the invention. In the following experimental examples, reagents, materials and equipment used in the methods are commercially available or conventionally prepared, unless otherwise specified, in order to make the technical scheme and features of the present invention more clear and understandable to those of ordinary skill in the art.
Example 1:
(1) taking 1 part of rose-flavored essence, 5 parts of methyl methacrylate, 0.03 part of sodium dodecyl sulfate, 0.1 part of azodiisobutyronitrile and 20 parts of deionized water in parts by mass, uniformly mixing, placing in a constant-temperature water bath kettle at 75 ℃, reacting for 10 hours under mechanical stirring at 300r/min, and taking out after cooling to obtain the aromatic seed microspheres coated with the polymethyl methacrylate essence.
(2) Taking 10 parts by mass of aromatic seed microspheres of polymethyl methacrylate-coated rose essence, 2 parts by mass of dopamine, 1 part by mass of tris (hydroxymethyl) aminomethane and 100 parts by mass of deionized water, uniformly mixing to obtain a reaction solution, determining the pH of the reaction solution to be 8.5, setting the reaction temperature to be 30 ℃, stirring the reaction solution at the stirring speed of 500r/min for 24 hours, and taking out to obtain the self-adhesive aromatic microcapsule with dopamine as a shell layer.
The obtained self-adhesive aromatic microcapsule is diluted by 10 times, cotton fabrics are finished in a padding-baking mode, the cotton fabrics are washed in water with the temperature of 50 ℃ for 30min for one time, and after the cotton fabrics are washed for 5 times, the cotton fabrics still have stronger rose aroma.
Example 2:
(1) taking 1 part of jasmine-flavored essence, 5 parts of methyl methacrylate, 0.03 part of hexadecyl trimethyl ammonium bromide, 0.1 part of benzoyl peroxide and 20 parts of deionized water in parts by mass, uniformly mixing, placing in a constant-temperature water bath kettle at 75 ℃, reacting for 10 hours under mechanical stirring at 300r/min, and taking out after cooling to obtain the polymethyl methacrylate-coated essence aromatic seed microspheres.
(2) Taking 10 parts by mass of aromatic seed microspheres of polymethyl methacrylate-coated jasmine essence, 2 parts of dopamine, 1 part of tris (hydroxymethyl) aminomethane and 100 parts of deionized water, uniformly mixing to obtain a reaction solution, determining the pH of the reaction solution to be 8.5, setting a reaction temperature of 30 ℃, stirring the reaction solution at a stirring speed of 500r/min for 24 hours, and taking out to obtain the self-adhesive aromatic microcapsule with dopamine as a shell layer.
The obtained self-adhesive aromatic microcapsule is diluted by 10 times, sprayed on napkin paper, and placed in a ventilated place after the napkin is dried, and the napkin paper still has strong jasmine aromatic smell after one week.
Example 3:
(1) taking 1 part by mass of lavender essence, 5 parts by mass of styrene, 0.03 part by mass of hexadecyltrimethylammonium chloride, 0.1 part by mass of benzoyl peroxide and 20 parts by mass of deionized water, uniformly mixing, placing in a constant-temperature water bath kettle at 75 ℃, reacting for 10 hours under mechanical stirring at 300r/min, and taking out after cooling to obtain the aromatic seed microspheres coated with the polystyrene essence.
(2) Taking 10 parts by mass of aromatic seed microspheres of the lavender essence coated by polystyrene, 2 parts by mass of dopamine, 1 part by mass of tris (hydroxymethyl) aminomethane and 100 parts by mass of deionized water, uniformly mixing to obtain a reaction solution, determining the pH of the reaction solution to be 8.5, setting the reaction temperature of 30 ℃, stirring the reaction solution at the stirring speed of 500r/min for 24 hours, and taking out to obtain the self-adhesive aromatic microcapsule with dopamine as a shell layer.
The obtained self-adhesive fragrant microcapsule is diluted by 10 times, and sprayed on a silk scarf, and after the scarf is washed for 3 times, the scarf still has a strong lavender fragrance.
Example 4:
(1) taking 1 part of cologne-flavored essence, 5 parts of styrene, 0.03 part of sodium dodecyl sulfate, 0.1 part of azodiisobutyronitrile and 20 parts of deionized water in parts by mass, uniformly mixing, placing in a constant-temperature water bath kettle at 75 ℃, reacting for 10 hours under mechanical stirring at 300r/min, and taking out after cooling to obtain the aromatic seed microspheres coated with the polystyrene essence.
(2) Taking 10 parts by mass of aromatic seed microspheres of polystyrene-coated rose essence, 2 parts by mass of dopamine, 1 part by mass of tris (hydroxymethyl) aminomethane and 100 parts by mass of deionized water, uniformly mixing to obtain a reaction solution, determining the pH of the reaction solution to be 8.5, setting the reaction temperature of 30 ℃, stirring the reaction solution at the stirring speed of 500r/min for 24 hours, and taking out to obtain the self-adhesive aromatic microcapsule with dopamine as a shell layer.
The obtained self-adhesive aromatic microcapsule is diluted by 10 times, is arranged in a transparent glass bottle, the glass bottle is opened and is placed in a ventilated place, and the microcapsule emulsion still has stronger cologne aromatic odor after one week.
The above is only a specific embodiment of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.
Claims (8)
1. A preparation method of self-adhesive aromatic microcapsules is characterized by comprising the following steps:
(1) the aromatic seed microspheres of polymer-coated essence are prepared by taking essence, organic monomers, an emulsifier, an oily initiator and deionized water as raw materials through an emulsion polymerization method, wherein the polymerization temperature is 75 ℃, and the reaction time is 10h
(2) The preparation method comprises the steps of preparing the self-adhesive aromatic microcapsule by taking aromatic seed microspheres of essence coated by a polymer, dopamine, trihydroxymethyl aminomethane and deionized water as raw materials, wherein the polymerization reaction temperature is 30 ℃, and the reaction time is 24 hours.
2. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: in the step (1), the mass of the organic monomer is 5 times of that of the essence, the mass ratio of the essence to the deionized water is 1:20, the emulsifier accounts for 3% of the mass of the essence, and the oily initiator accounts for 2% of the mass of the organic monomer.
3. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the essence in the step (1) is rose, lavender, jasmine and cologne-flavor essence.
4. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the organic monomer in the step (1) is one of methyl methacrylate and styrene.
5. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the emulsifier in the step (1) is one of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride and lauryl sodium sulfate.
6. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the oily initiator in the step (1) is one of azobisisobutyronitrile and benzoyl peroxide.
7. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: the aromatic seed microspheres in the step (2) account for 10% of the mass of the deionized water, the dopamine accounts for 2% of the mass of the deionized water, and the tris (hydroxymethyl) aminomethane accounts for 1% of the mass of the deionized water.
8. The process for the preparation of self-adhesive fragrant microcapsules according to claim 1, characterized in that: and (3) the pH value of the reaction liquid obtained after the raw materials are mixed in the step (2) is 8.5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112962320A (en) * | 2021-02-03 | 2021-06-15 | 浙江画之都文化创意有限公司 | Temperature-controlled fragrance-releasing particle and preparation method and application thereof |
| CN114085563A (en) * | 2021-12-28 | 2022-02-25 | 广东美涂士建材股份有限公司 | Green environment-friendly capsule release type antifouling paint and preparation method thereof |
| CN114808465A (en) * | 2022-03-10 | 2022-07-29 | 上海应用技术大学 | Textile perfuming-controllable self-adhesion microcapsule and preparation and application thereof |
| CN115572348A (en) * | 2022-09-28 | 2023-01-06 | 上海应用技术大学 | Preparation method of polydopamine methacrylamide lavender nanocapsule and application of polydopamine methacrylamide lavender nanocapsule in washing fastness |
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| CN114085563A (en) * | 2021-12-28 | 2022-02-25 | 广东美涂士建材股份有限公司 | Green environment-friendly capsule release type antifouling paint and preparation method thereof |
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| CN115572348A (en) * | 2022-09-28 | 2023-01-06 | 上海应用技术大学 | Preparation method of polydopamine methacrylamide lavender nanocapsule and application of polydopamine methacrylamide lavender nanocapsule in washing fastness |
| CN115572348B (en) * | 2022-09-28 | 2024-03-01 | 上海应用技术大学 | Preparation method of polydopamine methacrylamide lavender nanocapsules and application of polydopamine methacrylamide lavender nanocapsules in washing fastness |
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