CN102965196A - Preparation method of essential-oil-coated urea-modified melamine resin microcapsules - Google Patents
Preparation method of essential-oil-coated urea-modified melamine resin microcapsules Download PDFInfo
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- CN102965196A CN102965196A CN2012104456461A CN201210445646A CN102965196A CN 102965196 A CN102965196 A CN 102965196A CN 2012104456461 A CN2012104456461 A CN 2012104456461A CN 201210445646 A CN201210445646 A CN 201210445646A CN 102965196 A CN102965196 A CN 102965196A
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Abstract
The invention discloses a preparation method of essential-oil-coated urea-modified melamine resin microcapsules, which comprises the following steps: (1) wall material pre-crosslinking: by using a melamine-formaldehyde prepolymer as a wall material and urea as a modifier, carrying out pre-crosslinking to obtain a pre-crosslinked wall material solution; (2) core material emulsification: by using essential oil as a core material, forming an oil-in-water emulsion with the pre-crosslinked wall material solution; (3) capsule wall formation: stirring the oil-in-water emulsion to form capsule walls; and (4) termination of crosslinking reaction: adding an alkali solution to terminate the crosslinking reaction. The essential-oil-coated urea-modified melamine resin microcapsules prepared according to the method disclosed by the invention has the advantages of enhanced toughness, lower brittleness and improved storage stability, and slow release of the essential-oil in the microcapsules is facilitated; and the essential-oil-coated urea-modified melamine resin microcapsules have low formaldehyde residue level and favorable dispersity in the water-based solution system, and thus, is beneficial to application in washing agents and the like.
Description
Technical field
The present invention relates to the microcapsulary field, particularly a kind of preparation method who coats the urea modification melamine resin microcapsule of volatile oil.
Background technology
Material of microencapsulation technology permission is encapsulated in one and has size ranges in one micron microballoon or micro-capsule that arrives between the hundreds of micron.This technology has been widely used in many-sided application such as medicine, agricultural, food, printing, makeup, daily use chemicals.
Along with the raising of expanding economy and people's living standard, people are greatly improved to the requirement of washing composition.When pursuing practical value, also change to enjoyment, health direction gradually.In washing composition, add volatile oil and can make clothing etc. keep fragrance, can make the clothing anti-bacteria growth, covering smell, make people's body and mind comfortable.Yet volatile oil is unfavorable for the reservation of washing composition fragrance because volatility is very strong.Utilize microcapsulary, the volatile oil micro encapsulation joined to guarantee in the washing composition that volatile oil is stable in storage process, on the other hand, in washing process, the microcapsule that partly coat volatile oil break through the washing extruding volatile oil are discharged, perhaps stick to and continue in the clothes fiber slowly to discharge volatile oil, make clothing keep for a long time fragrance.
Melamine resin has good film-forming quality owing to cheap, therefore is widely used in the preparation of microcapsule.But melamine resin makes the microcapsule of preparation have the shortcomings such as poor toughness, fragility is high, package stability is poor because of its unique triazine ring and the interlaced structure of methylol.In addition, because preparation process used formaldehyde, its residual quantity control ratio is difficult, and all this is allly restricting the application of microcapsule in washing composition.Mean in the washing composition that for coating the microcapsule of volatile oil, joining stronger toughness and physical strength need to be arranged, the stability requirement of storing simultaneously is also higher.Therefore, need to be by melamine resin being carried out to a certain degree modification to improve its mechanical property and releasing properties.
Summary of the invention
In order to overcome the above-mentioned shortcoming and defect of prior art, the object of the present invention is to provide a kind of preparation method who coats the urea modification melamine resin microcapsule of volatile oil, improved the mechanical property such as toughness, fragility of melamine resin microcapsule, improve the compactness of microcapsule, prolong the time of releasing of volatile oil, improved package stability.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method who coats the urea modification melamine resin microcapsule of volatile oil may further comprise the steps:
(1) wall material precrosslink: take the carbamide prepolymer as the wall material, take urea as properties-correcting agent, carry out precrosslink, obtain the wall material solution after the precrosslink;
(2) core emulsification: take volatile oil as core, with the wall material solution formation O/w emulsion after the precrosslink;
(3) cyst wall forms: stir O/w emulsion, form cyst wall;
(4) stop crosslinking reaction: add alkaline solution and stop crosslinking reaction.
The described wall material of step (1) precrosslink: take the carbamide prepolymer as the wall material, take urea as properties-correcting agent, carry out precrosslink, obtain the wall material solution after the precrosslink, be specially:
The deionized water that in the dispersion agent of per 1.2 ~ 2.1g, adds 120 ~ 160g, regulating pH is 8.0 ~ 9.0, with dispersion agent emulsification 2h, is cooled to room temperature under 30 ~ 50 ℃ of conditions;
Add 6.5 ~ 17.2g solid holdup and be 24 ~ 50%, residual formaldehyde is lower than 0.2% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.18 ~ 0.32g; The urea that adds again 0.5 ~ 1.0g; Then regulate pH=3.5 ~ 4.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 300 ~ 600rpm stirs 105 ~ 150min; Described carbamide prepolymer with trimeric cyanamide and formaldehyde mass ratio in 1:(0.4 ~ 6) preparation.
The described core emulsification of step (2): take volatile oil as core, form O/w emulsion with the wall material solution after the precrosslink, be specially: the wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.3 ~ 0.9g emulsifying agent, 0.2 ~ 0.6g defoamer, again regulating the pH value is 3.5 ~ 4.5; Then, add the volatile oil of 12.0 ~ 18.0g, in ice-water bath, regulate mulser rotating speed 1200 ~ 3000rpm, emulsification 30 ~ 40min forms O/w emulsion.
The described cyst wall of step (3) forms: stir O/w emulsion, form cyst wall, be specially:
O/w emulsion is stirred 30 ~ 40min with 300 ~ 600rpm speed at ambient temperature; Then, 6 ~ 7h is stirred with 300 ~ 600rpm speed in rising temperature to 65 ~ 75 ℃.
The described termination crosslinking reaction of step (4) adds alkaline solution and stops crosslinking reaction, is specially:
The product that step (3) is obtained is cooled to room temperature, regulates pH=10 ~ 11 with the yellow soda ash dilute solution, stops crosslinking reaction.
The described dispersion agent of step (1) be in vinylformic acid copolymer-maleic anhydride, Zelan 338 and the acrylamide-sodium acrylate copolymer any one or two or more.
The described emulsifying agent of step (2) be in the alkylphenol polyoxyethylene (OP-10) that contains 10 carbon atoms, Sorbitan ethoxylate (Tween-80), the polyoxyethylene carboxylate any one or two or more.
The described defoamer of step (2) is arbitrary component in propyl carbinol, tributyl phosphate, the water-based silicone oil or two or more.
The described emulsifying kettle of step (2) adopts the 304# stainless steel to make, and internal diameter is 90mm, and wall thickness is 5mm, and the emulsifying kettle inwall is welded with 3 baffle plates that are evenly distributed; The level cross-sectionn of described baffle plate is that central angle is 30 °, and radius is the fan-shaped of 8mm.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) to prepare microcapsule capsule wall material cheap and easy to get in the present invention, preparation condition realizes easily, reduced the cost that preparation coats the volatile oil microcapsule, is conducive to the large-scale production of this technology.
(2) emulsion process of the present invention adopts the stainless steel emulsifying kettle of autonomous design, by adding three baffle plates, reduces widely whirlpool, increases the mutual collision frequency of drop.Simultaneously, added baffle plate, the emulsification shearing force acts on the drop more equably, and the emulsion droplet size-grade distribution that obtains is also more even.
(3) the present invention adopts urea modification melamine resin to prepare microcapsule, has strengthened the toughness of microcapsule, has reduced fragility, has also improved the package stability of microcapsule simultaneously, is conducive to the slow release of volatile oil in the microcapsule.
(4) the present invention strictly controls the amount that adds formaldehyde, and monitors the microcapsule residual formaldehyde for preparing, and the microcapsule residual formaldehyde for preparing is lower than prescribed minimum.
(5) the urea modification melamine resin microcapsule of the coating volatile oil of the present invention's preparation have preferably dispersiveness in aqueous solvent, are conducive to its application in washing composition.
Description of drawings
Fig. 1 is the synoptic diagram of the emulsifying kettle of embodiments of the invention 1 employing.
Fig. 2 is the level cross-sectionn figure of Fig. 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Add 1.2g dispersion agent vinylformic acid copolymer-maleic anhydride in the 250mL round-bottomed flask, the deionized water of 160g is regulated pH=8.0 with 10% massfraction NaOH solution, with dispersion agent emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the 17.2g solid holdup and be 24%, residual formaldehyde is 0.19% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.18g; The urea that adds again 0.84g; Then regulate pH=4.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 300rpm stirs 105min; Described carbamide prepolymer prepares at 1:0.4 with trimeric cyanamide and formaldehyde mass ratio.Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.9g emulsifier op-10,0.6g defoamer propyl carbinol, again regulating the pH value is 4.5.Then, add 18.0g volatile oil, in ice-water bath, regulate mulser rotating speed 1200rpm, emulsification 30min forms O/w emulsion.
The emulsion that obtains is poured in the 250mL round-bottomed flask, stirred 30min with 300rpm speed under the room temperature condition.Then, rising temperature to 65 ℃ stirred 6 hours with 300rpm speed.
The product that stirring was obtained after 6 hours is cooled to room temperature, with 10% massfraction Na
2CO
3Regulate pH=10, stop crosslinking reaction.
Shown in Fig. 1 ~ 2, the emulsifying kettle that present embodiment adopts is made by the 304# stainless steel, and internal diameter is 90mm, and wall thickness is 5mm, and the emulsifying kettle inwall is welded with 3 baffle plates 1 that are evenly distributed; The level cross-sectionn of described baffle plate 1 is that central angle is 30 °, and radius is the fan-shaped of 8mm.
Be residual formaldehyde in the urea modification melamine resin microcapsule of measuring the coating volatile oil for preparing, adopt phenol reagent spectrophotometry (GB/18204.26-2000) to measure.
Be the median size of the urea modification melamine resin microcapsule of the coating volatile oil of measuring preparation, adopt microcapsule that observation by light microscope makes and its size size-grade distribution is added up, obtain the mean sizes of microcapsule.
Encapsulation ratio for the urea modification melamine resin microcapsule of the coating volatile oil of measuring preparation adopts thermogravimetric analysis roughly to determine the encapsulation ratio of microcapsule.
For the roughly rate of release of the urea modification melamine resin microcapsule of the coating volatile oil of measuring preparation, will in 30 ℃ of baking ovens, place 15 days after the microcapsule drying, the changes in weight before and after weighing is placed is calculated residual mass percent.
Measurement result is as shown in table 1.
Embodiment 2
Embodiment 2 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
Add 1.7g dispersion agent Zelan 338 in the 250mL round-bottomed flask, the deionized water of 140g is regulated pH=8.0 with 10%NaOH solution, with dispersion agent emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the 10g solid holdup and be 36%, residual formaldehyde is 0.14% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.26g; The urea that adds again 0.7g; Then regulate pH=4.3 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 600rpm stirs 150min; Described carbamide prepolymer prepares at 1:2.5 with trimeric cyanamide and formaldehyde mass ratio.
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.4g emulsifier op-10,0.3g defoamer water-based silicone oil, again regulating the pH value is 4.3.Then, add 15.0g volatile oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min forms O/w emulsion.
The emulsion that obtains is poured in the 250mL round-bottomed flask, stirred 40min with 600rpm speed under the room temperature condition.Then, rising temperature to 75 ℃ stirred 7 hours with 600rpm speed.
The product that stirring was obtained after 7 hours is cooled to room temperature, with 10% massfraction Na
2CO
3Regulate pH=11, stop crosslinking reaction.
Determination step is identical with embodiment 1, and measurement result is as shown in table 1.
Embodiment 3
Embodiment 3 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
Add 2.1g acrylamide-sodium acrylate copolymer dispersion agent in the 250mL round-bottomed flask, the deionized water of 120g is regulated pH=9.0 with 10% massfraction NaOH solution, with dispersion agent emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the 6.5g solid holdup and be 50%, residual formaldehyde is 0.15% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.18g; The urea that adds again 0.5g; Then regulate pH=3.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 500rpm stirs 120min; Described carbamide prepolymer prepares at 1:6 with trimeric cyanamide and formaldehyde mass ratio.
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.3g emulsifying agent Tween-80,0.2g defoamer propyl carbinol, again regulating the pH value is 3.5.Then, add 12.0g volatile oil, in ice-water bath, regulate mulser rotating speed 3000rpm, emulsification 40min forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 4
Embodiment 4 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
(wherein the vinylformic acid copolymer-maleic anhydride is 1g to add the mixture of 1.7g vinylformic acid copolymer-maleic anhydride and acrylamide-sodium acrylate copolymer in the 250mL round-bottomed flask, acrylamide-sodium acrylate copolymer is 0.7g) as dispersion agent, the deionized water of 140g, regulate pH=8.0 with 10% massfraction NaOH solution, under 50 ℃ of conditions, with dispersion agent emulsification 2h, be cooled to room temperature.Add the 7.2g solid holdup and be 50%, residual formaldehyde is 0.2% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.26g; The urea that adds again 0.9g; Then regulate pH=4.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 300rpm stirs 150min; Described carbamide prepolymer prepares at 1:3 with trimeric cyanamide and formaldehyde mass ratio.
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.4g emulsifying agent polyoxyethylene carboxylate, 0.3g defoamer tributyl phosphate, again regulating the pH value is 4.3.Then, add 15.0g volatile oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 5
Embodiment 5 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.5g emulsifier op-10,0.4g defoamer propyl carbinol, again regulating the pH value is 4.3.Then, add 15.0g volatile oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 6
Embodiment 6 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
(wherein Zelan 338 is 0.5g to add the mixture of 1.9g Zelan 338, vinylformic acid copolymer-maleic anhydride and acrylamide-sodium acrylate copolymer in the 250mL round-bottomed flask, the vinylformic acid copolymer-maleic anhydride is 1g, acrylamide-sodium acrylate copolymer is 0.4g) dispersion agent, the deionized water of 140g, regulate pH=8.0 with 10% massfraction NaOH solution, under 50 ℃ of conditions, with dispersion agent emulsification 2h, be cooled to room temperature.Add the 7.2g solid holdup and be 50%, residual formaldehyde is 0.2% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.26g; The urea that adds again 0.7g; Then regulate pH=4.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 600rpm stirs 150min; Described carbamide prepolymer prepares at 1:3 with trimeric cyanamide and formaldehyde mass ratio.
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.5g emulsifier op-10,0.4g defoamer propyl carbinol, again regulating the pH value is 4.3.Then, add 15.0g volatile oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 7
Embodiment 7 prepares the urea modification melamine resin microcapsule that coat volatile oil according to the following steps:
Add 1.7g vinylformic acid copolymer-maleic anhydride dispersion agent in the 250mL round-bottomed flask, the deionized water of 140g is regulated pH=8.0 with 10% massfraction NaOH solution, with dispersion agent emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the 7.2g solid holdup and be 50%, residual formaldehyde is 0.2% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.26g; The urea that adds again 0.5 ~ 1.0g; Then regulate pH=3.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 300rpm stirs 150min; Described carbamide prepolymer prepares at 1:3 with trimeric cyanamide and formaldehyde mass ratio.
Wall material solution after the precrosslink is poured in the emulsifying kettle, added 0.4g emulsifier op-10,0.3g defoamer propyl carbinol, again regulating the pH value is 4.3.Then, add 15.0g volatile oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Each embodiment location parameter of table 1
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not limited by the examples; can be for containing the alkylphenol polyoxyethylene of 10 carbon atoms such as emulsifying agent; Sorbitan ethoxylate; two or more mixture in the polyoxyethylene carboxylate; defoamer can be propyl carbinol; tributyl phosphate; two or more mixture in the water-based silicone oil etc.; other any do not deviate from the change of doing under spirit of the present invention and the principle; modify; substitute; combination; simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a preparation method who coats the urea modification melamine resin microcapsule of volatile oil is characterized in that, may further comprise the steps:
(1) wall material precrosslink: take the carbamide prepolymer as the wall material, take urea as properties-correcting agent, carry out precrosslink, obtain the wall material solution after the precrosslink;
(2) core emulsification: take volatile oil as core, with the wall material solution formation O/w emulsion after the precrosslink;
(3) cyst wall forms: stir O/w emulsion, form cyst wall;
(4) stop crosslinking reaction: add alkaline solution and stop crosslinking reaction.
2. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 1, it is characterized in that, the described wall material of step (1) precrosslink: take the carbamide prepolymer as the wall material, take urea as properties-correcting agent, carry out precrosslink, obtain the wall material solution after the precrosslink, be specially:
The deionized water that in the dispersion agent of per 1.2 ~ 2.1g, adds 120 ~ 160g, regulating pH is 8.0 ~ 9.0, with dispersion agent emulsification, is cooled to room temperature under 30 ~ 50 ℃ of conditions;
Add 6.5 ~ 17.2g solid holdup and be 24 ~ 50%, residual formaldehyde is lower than 0.2% carbamide prepolymer; Add formaldehyde solution, the formaldehyde total content that makes adding is 0.18 ~ 0.32g; The urea that adds again 0.5 ~ 1.0g; Then regulate pH=3.5 ~ 4.5 with dilute solution of acetic acid, at ambient temperature, adjusting rotary speed 300 ~ 600rpm stirs 105 ~ 150min; Described carbamide prepolymer with trimeric cyanamide and formaldehyde mass ratio in 1:(0.4 ~ 6) preparation.
3. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 1, it is characterized in that, the described core emulsification of step (2): take volatile oil as core, form O/w emulsion with the wall material solution after the precrosslink, be specially: the wall material solution after the precrosslink is poured in the emulsifying kettle, add 0.3 ~ 0.9g emulsifying agent, 0.2 ~ 0.6g defoamer, again regulating the pH value is 3.5 ~ 4.5; Then, add the volatile oil of 12.0 ~ 18.0g, in ice-water bath, regulate mulser rotating speed 1200 ~ 3000rpm, emulsification 30 ~ 40min forms O/w emulsion.
4. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 1 is characterized in that, the described cyst wall of step (3) forms: stir O/w emulsion, form cyst wall, be specially:
O/w emulsion is stirred 30 ~ 40min with 300 ~ 600rpm speed at ambient temperature; Then, 6 ~ 7h is stirred with 300 ~ 600rpm speed in rising temperature to 65 ~ 75 ℃.
5. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 1 is characterized in that, the described termination crosslinking reaction of step (4) adds alkaline solution and stops crosslinking reaction, is specially:
The product that step (3) is obtained is cooled to room temperature, regulates pH=10 ~ 11 with the yellow soda ash dilute solution, stops crosslinking reaction.
6. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 2, it is characterized in that, the described dispersion agent of step (1) be in vinylformic acid copolymer-maleic anhydride, Zelan 338 and the acrylamide-sodium acrylate copolymer any one or two or more.
7. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 3, it is characterized in that, the described emulsifying agent of step (2) be in the alkylphenol polyoxyethylene that contains 10 carbon atoms, Sorbitan ethoxylate, the polyoxyethylene carboxylate any one or two or more.
8. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 3 is characterized in that, the described defoamer of step (2) is arbitrary component in propyl carbinol, tributyl phosphate, the water-based silicone oil or two or more.
9. the preparation method of the urea modification melamine resin microcapsule of coating volatile oil according to claim 3, it is characterized in that the described emulsifying kettle of step (2) adopts the 304# stainless steel to make, internal diameter is 90mm, wall thickness is 5mm, and the emulsifying kettle inwall is welded with 3 baffle plates that are evenly distributed; The level cross-sectionn of described baffle plate is that central angle is 30 °, and radius is the fan-shaped of 8mm.
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| CN103769020A (en) * | 2014-01-21 | 2014-05-07 | 华南理工大学 | Dual-core microcapsule, preparation method and application thereof |
| CN107709535A (en) * | 2015-05-29 | 2018-02-16 | 宝洁公司 | Fluid fabric intensifier composition |
| CN107835707B (en) * | 2015-07-02 | 2021-09-14 | 奇华顿股份有限公司 | Microcapsules |
| KR20180023962A (en) * | 2015-07-02 | 2018-03-07 | 지보당 에스아 | Microcapsule |
| CN107835707A (en) * | 2015-07-02 | 2018-03-23 | 奇华顿股份有限公司 | Microcapsules |
| US10537868B2 (en) | 2015-07-02 | 2020-01-21 | Givaudan S.A. | Microcapsules |
| CN113170920A (en) * | 2020-01-08 | 2021-07-27 | 中国科学院理化技术研究所 | Temperature-control heat-conducting multifunctional microcapsule for cigarettes and preparation method thereof |
| CN112841184A (en) * | 2021-01-28 | 2021-05-28 | 常州大学 | Physcion microcapsule sustained release agent and preparation method thereof |
| CN113999726A (en) * | 2021-08-18 | 2022-02-01 | 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 |
| 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 |
| CN113713726A (en) * | 2021-09-10 | 2021-11-30 | 国家林业和草原局竹子研究开发中心 | Mildew-proof microcapsule for bamboo wood and preparation method thereof |
| CN113713726B (en) * | 2021-09-10 | 2024-04-30 | 国家林业和草原局竹子研究开发中心 | Mildew-proof microcapsule for bamboo wood and preparation method thereof |
| CN115430371A (en) * | 2022-06-29 | 2022-12-06 | 上海宾佑新材料科技有限公司 | Meyer sedge essential oil microcapsule, preparation method and application |
| CN116116331A (en) * | 2023-01-06 | 2023-05-16 | 华南理工大学 | Epoxy resin microcapsule and preparation method and application thereof |
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