CN102513045A - Water-soluble fragrance microcapsule having slow release characteristics and preparation method thereof - Google Patents
Water-soluble fragrance microcapsule having slow release characteristics and preparation method thereof Download PDFInfo
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- CN102513045A CN102513045A CN2011104306559A CN201110430655A CN102513045A CN 102513045 A CN102513045 A CN 102513045A CN 2011104306559 A CN2011104306559 A CN 2011104306559A CN 201110430655 A CN201110430655 A CN 201110430655A CN 102513045 A CN102513045 A CN 102513045A
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Abstract
The invention provides a water-soluble fragrance microcapsule having slow release characteristics and a preparation method thereof. A capsule core of the microcapsule is porous starch having adsorbed oil-soluble essential oil, and a capsule wall is water-soluble polyethylene glycol. The microcapsule does not release fragrance when the microcapsule does not contact with aqueous liquid like body fluid and has good storage performance; when the microcapsule contacts with aqueous liquid, the water-soluble capsule wall at the exterior of the microcapsule is dissolved in the aqueous liquid, so capsule core substances having fragrance permeate micropores in the porous starch at an internal layer and are slowly released, thereby achieving the goals of lasting shielding of stink and removal of a peculiar smell. In the preparation process of the microcapsule, loss of the fragrant substances is small, the preparation method is simple and is suitable for industrial production, and an absorbent resin is endowed with special deodorizing capability when the absorbent resin is combined with the microcapsule.
Description
Technical field
The present invention relates to a kind of water-soluble aromatic microcapsules and preparation method thereof with slow release characteristic; More specifically; When the present invention relates to a kind of absorber that is used for hygienic material; Thereby have the preparation method that lasting release aromatic substance plays the water-soluble aromatic microcapsules that cover stink (peculiar smell) effect, belong to the microcapsules preparing technical field.
Background technology
In water-absorbing resin, add aromatic substance, can make water-absorbing resin when absorbing body fluid (like urine), give out fragrance, thereby cover the stink of urine, solid feces etc., play the effect of deodorizing.Yet the boiling point of aromatic substance is lower, after mixing with water-absorbing resin, can not store for a long time.Through aromatic substance microencapsulations such as essence being provided the shell of a protectiveness to essence, shield it and contact with the direct of outside air or product, effectively stop essence volatilization, react or be diffused into and add in the incense products.
Yet compare with the microcapsules technology of other core; The microencapsulation difficulty of essence is bigger; This mainly be because: normally tens kinds in (1) essence; Even the mixture of hundreds of different component, they have nothing in common with each other to the dissolubility of water with oil, and it is very difficult therefore will all components being embedded in the wall material fully; (2) different component in the essence has different boiling, and component volatilization property difference is big, even some components still have very strong volatility below 0 ℃, the volatilization loss of volatile component causes the variation of odor type; (3) the many components of essence are to pH, light, heat, oxygen sensitivity, and making has brought difficulty to microcapsules.Especially, for the aromatic micro-capsule that is applied to the water-absorbing resin system, require microcapsules in air, to have good compactness and make it can long term storage, in case and contact with water can dissolve rapidly and discharge aromatic substance.The method for preparing at present essence microcapsule mainly contains spray drying process, situ aggregation method, complex coacervation, extrusion etc.As far as the preparation water soluble microcapsule,, therefore select for use spray drying process, cyclodextrin encapsulated method, extrusion to wait and prepare usually because it is water-soluble to require the wall material of microcapsules to have.As in Chinese patent CN1680519,101889673A, 02208802, having put down in writing the method that adopts the spray drying method for preparation water soluble microcapsule; Disclose a kind of method with the white inclusion resveratrol of hydroxypropyl microcapsules among the Chinese patent CN201010238853.0, the microcapsules tool of preparation is that white powder has water-quick-soluble.Yet for coating aromatic substance; All there are some limitation in the above-mentioned several kinds of technologies that prepare water soluble microcapsule; Handle through the hot blast of high temperature as needing in the drying process with atomizing, therefore will make some the low-boiling point material volatilizations in the volatile oil, thereby influence the smell of microcapsule product.And the clad ratio of beta-cyclodextrin inclusion compound technology is lower and the little material of cavity that can only the cladding ratio cyclodextrin, thereby its application also is restricted.
Summary of the invention
The purpose of this invention is to provide a kind of water-soluble aromatic microcapsules and preparation side thereof,, satisfy the needs of the parties concerned to overcome the above-mentioned defective that prior art exists with slow release characteristic.
Described water-soluble aromatic microcapsules with slow release characteristic, capsule-core is the porous-starch that is adsorbed with the oil-soluble volatile oil, and cyst wall is water miscible polyethylene glycol, and particle diameter is 200-300 μ m;
In the gross weight of capsule-core, the weight of volatile oil is 5-40%;
Porous-starch is the 25-60% of polyethylene glycol weight;
The preferred crystallization temperature of said polyethylene glycol is 40～65 ℃ a polyethylene glycol;
Described porous-starch is a kind of novel converted starch, and it is that the enzyme with living amylase activity is being lower than the cellular product of porous that acts on living starch under the gelatinization point and form.Can adopt commercially produced product, be the product of smart crystallographic system row like Liaoning Rieter bio tech ltd company trade mark, perhaps adopts the method for (preparation of porous-starch and character-permitted Li Na Shandong Agricultural University Master's thesis 2009) research reported in literature to prepare;
Described oil-soluble volatile oil does not have special requirement, more than one in preferred lemon, orange essential oil or the Rosa Damascana;
Prepare described method, comprise the steps: with water-soluble aromatic microcapsules of slow release characteristic
(1) with porous-starch, under stirring condition, mix with the oil-soluble volatile oil, be adsorbed onto in the how empty starch with making the oil-soluble essential oil, obtain to have adsorbed the porous-starch of oil-soluble volatile oil, be capsule-core;
(2) with the polyethylene glycol heating and melting; Then under stirring condition, in the polyethylene glycol of fusion, add step (1) preparation absorption the porous-starch of oil-soluble volatile oil, disperse; Product after will disperseing then is cooled to below 25 ℃; The polyethylene glycol cooled and solidified, it is crushed to particle diameter is 200～300 μ m, obtains described water-soluble aromatic microcapsules with slow release characteristic;
Wherein, to account for the quality of polyethylene glycol be 25-60% to porous-starch.
The capsule-core of the microcapsules that the present invention relates to; For being adsorbed with the porous-starch of volatile oil; Cyst wall is water miscible polyethylene glycol, when contacting waterborne liquids such as body fluid, does not discharge aromatic odor when microcapsules like this, has good storage performance; And when these microcapsules in contact during waterborne liquid; The outside water-soluble cyst wall of microcapsules dissolves in waterborne liquid, has slowly releasing of micropore on the capsule-core material permeance internal layer porous-starch of aromatic odor like this in the microcapsules, thereby plays the purpose of covering stink lastingly, eliminating the unusual smell.The invention has the beneficial effects as follows:
In the process of microcapsules preparation, the aromatic substance loss is less, and preparation technology is simple, is suitable for suitability for industrialized production, after with these microcapsules and water-absorbing resin combination, can give water-absorbing resin special deodorizing capability.
The specific embodiment
Embodiment 1
(1) mixing the porous-starch that machine adds 500g, the oil factor＞1.5g/g of starch.The oil-soluble lemon extract that under stirring condition, in batches adds 100g makes essence be adsorbed onto in the porous-starch equably;
(2) the 1000g Macrogol 6000 is added in the stirred tank of band heater; Being heated to 80 ℃ melts polyethylene glycol fully; Under stirring condition, in the polyethylene glycol of fusion, add the prepared porous-starch that adsorbs essential oil of step (1); Stir fast how empty starch is evenly disperseed in polyethylene glycol, this mixed liquor is poured into fast in the uncovered dish and is cooled off below 25 ℃ naturally then, treat the complete cooled and solidified of polyethylene glycol of coated porous starch after; It is crushed to average grain diameter is 220 μ m, thereby obtains having the water-soluble aromatic microcapsules of slow release characteristic.
Embodiment 2
Among the embodiment 1, the lemon extract in the step 1 is changed to flavoring rose essence, all the other are with embodiment 1.The particle diameter of product is 200-300 μ m.
Embodiment 3
Among the embodiment 1, the Macrogol 6000 in the step 2 is changed to Macrogol 2000, all the other are with embodiment 1.The average grain diameter of product is 300 μ m.
Embodiment 4
(1) mixing the porous-starch that machine adds 500g, the oil factor＞1.5g/g of starch.The oil-soluble lemon extract that under stirring condition, in batches adds 200g makes essence be adsorbed onto in the porous-starch equably;
(2) the 2500g Macrogol 6000 is added in the stirred tank of band heater; Being heated to 80 ℃ melts polyethylene glycol fully; Under stirring condition, in the polyethylene glycol of fusion, add the prepared porous-starch that adsorbs essential oil of step (1); Stir fast how empty starch is evenly disperseed in polyethylene glycol, this mixed liquor is poured into fast in the uncovered dish and is cooled off below 25 ℃ naturally then, treat the complete cooled and solidified of polyethylene glycol of coated porous starch after; It is crushed to particle diameter 200-300 μ m, thereby obtains having the water-soluble aromatic microcapsules of slow release characteristic.The average grain diameter of product is 240 μ m.
Comparative Examples 1
At the porous-starch of high-speed mixing machine adding 1500g, the oil factor＞1.5g/g of starch.Under stirring condition, add the lemon extract (oil-soluble) of 100g in batches, essence is adsorbed onto in the porous-starch equably, obtain adsorbing the porous-starch of essence.The average grain diameter of product is 300 μ m.
Comparative Examples 2
The 1500g Macrogol 6000 is added in the stirred tank of band heater; Be heated to 80 ℃ polyethylene glycol melted fully, under stirring condition in the polyethylene glycol of fusion 100g lemon extract (oil-soluble), stir fast essence evenly disperseed in polyethylene glycol; This mixed liquor is poured cooling naturally in the uncovered dish fast into then; After waiting to coat the complete cooled and solidified of polyethylene glycol of essence, it is crushed to required particle diameter, thereby obtains water soluble microcapsule.The average grain diameter of product is 220 μ m.
In order to simulate prepared aromatic micro-capsule in actual use to the screening performance of stink, it is that the water-absorbing resin of ZNK is tested the screening performance of peculiar smell prepared aromatic micro-capsule that the present invention adopts the Jinan Wu Yue resin Co., Ltd trade mark.Before the test, earlier the aromatic micro-capsule of different process preparation is placed 24h in ventilated environment and test again.
Method of testing is following: in the glass beaker of 150ml capacity, put into the 1g testing sample, add the 10g infant urine then, trained and qualifiedly smell the person of distinguishing and carry out artificial sense of smell evaluation in different time intervals by 1.Oder levels is divided into: giving off a strong fragrance flavor, light fragrance, tasteless, slight peculiar smell, peculiar smell, dense peculiar smell are six types slightly, add up according to the evaluation result of smelling the person of distinguishing.Experimental result is seen table 1.
Smell over time after table 1 water-absorbing resin/aromatic micro-capsule composition added urine
Can find out from the experimental result of table 1; Single starch absorption essence (Comparative Examples 1) and wrap up covering the time of stink that essence (Comparative Examples 2) produces urine with polyethylene glycol; Be significantly shorter than microcapsules (embodiment 1) with double-deck cyst wall; And after the essence process coated with polyethylene glycol, its speed that in air, discharges is slowed down.This explanation is adsorbed onto the rate of release that can control essence in the porous-starch effectively with essence; And can prevent effectively that through outside the porous-starch of absorption essence, coating the water miscible polyethylene glycol of one deck essence from discharging to the external world in storage, thereby prolong the memory time of essence microcapsule.
Claims (7)
1. have the water-soluble aromatic microcapsules of slow release characteristic, it is characterized in that, capsule-core is the porous-starch that is adsorbed with the oil-soluble volatile oil, and cyst wall is water miscible polyethylene glycol.
2. the water-soluble aromatic microcapsules with slow release characteristic according to claim 1 is characterized in that, particle diameter is 200-300 μ m.
3. the water-soluble aromatic microcapsules with slow release characteristic according to claim 1 and 2 is characterized in that, in the gross weight of capsule-core, the weight of volatile oil is 5-40%, and porous-starch is the 25-60% of polyethylene glycol weight.
4. the water-soluble aromatic microcapsules with slow release characteristic according to claim 3 is characterized in that, the preferred crystallization temperature of said polyethylene glycol is 40～65 ℃ a polyethylene glycol.
5. the water-soluble aromatic microcapsules with slow release characteristic according to claim 4 is characterized in that, described oil-soluble volatile oil is more than one in lemon, orange essential oil or the Rosa Damascana.
6. each described method with water-soluble aromatic microcapsules of slow release characteristic of claim 1～5 is asked in preparation, it is characterized in that, comprises the steps:
(1) with porous-starch, under stirring condition, mix with the oil-soluble volatile oil, be adsorbed onto in the how empty starch with making the oil-soluble essential oil, obtain to have adsorbed the porous-starch of oil-soluble volatile oil, be capsule-core;
(2) with the polyethylene glycol heating and melting; Then under stirring condition, in the polyethylene glycol of fusion, add step (1) preparation absorption the porous-starch of oil-soluble volatile oil, disperse; Product after will disperseing then is cooled to below 25 ℃; The polyethylene glycol cooled and solidified, it is crushed to particle diameter is 200～300 μ m, obtains described water-soluble aromatic microcapsules with slow release characteristic.
7. method according to claim 6 is characterized in that, the quality that porous-starch accounts for polyethylene glycol is 25-60%.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776068A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Paste type microcapsule flavoring rose essence and preparation method thereof |
| CN102776070A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Transparent microcapsule flavoring rose essence and preparation method thereof |
| CN102965196A (en) * | 2012-11-09 | 2013-03-13 | 华南理工大学 | Preparation method of essential-oil-coated urea-modified melamine resin microcapsules |
| CN103598178A (en) * | 2013-10-25 | 2014-02-26 | 浙江理工大学 | Preparation method of insect-protected starch slow release microspheres |
| CN106189497A (en) * | 2016-08-29 | 2016-12-07 | 苏州安洁科技股份有限公司 | A kind of spacetabs type fragrance water color ink |
| CN106491374A (en) * | 2016-12-06 | 2017-03-15 | 广州睿森生物科技有限公司 | A kind of nepetalactone microcapsule and preparation method thereof with preparing the application in mosquito repellent product |
| CN106753898A (en) * | 2017-01-06 | 2017-05-31 | 南京福科帝生物科技有限公司 | A kind of odor prolongation clothes washing compositions of additives containing porous-starch and preparation method thereof |
| CN108354000A (en) * | 2018-04-19 | 2018-08-03 | 西安工程大学 | Fresh-keeping for fresh agricultural products slow, released microcapsule and preparation method thereof |
| CN110623076A (en) * | 2019-10-17 | 2019-12-31 | 湖北文理学院 | Instant walnut food containing rose essential oil and preparation method thereof |
| CN110982620A (en) * | 2019-11-26 | 2020-04-10 | 云南中烟工业有限责任公司 | Porous starch-loaded molecular capsule, and preparation method and application thereof |
| CN111560771A (en) * | 2019-05-24 | 2020-08-21 | 安徽农业大学 | Embroidery anticorrosion and antioxidation method for three-dimensional pattern |
| CN111820394A (en) * | 2020-09-21 | 2020-10-27 | 鲁东大学 | Preparation method of slow-release Chinese torreya shell essence |
| CN114405423A (en) * | 2022-01-11 | 2022-04-29 | 广州乐居日化用品有限公司 | Porous chitosan microcapsule fragrance retaining bead and high-stability laundry gel bead |
| WO2022126913A1 (en) * | 2020-12-17 | 2022-06-23 | 天津春发生物科技集团有限公司 | Method for preparing liquid-type microcapsule product having flowability |
| CN114711411A (en) * | 2022-03-31 | 2022-07-08 | 重庆小丸生物科技股份有限公司 | Self-dispersed oil microcapsule in water and preparation method thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776070A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Transparent microcapsule flavoring rose essence and preparation method thereof |
| CN102776068A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Paste type microcapsule flavoring rose essence and preparation method thereof |
| CN102965196A (en) * | 2012-11-09 | 2013-03-13 | 华南理工大学 | Preparation method of essential-oil-coated urea-modified melamine resin microcapsules |
| CN102965196B (en) * | 2012-11-09 | 2014-05-07 | 华南理工大学 | Preparation method of essential-oil-coated urea-modified melamine resin microcapsules |
| CN103598178A (en) * | 2013-10-25 | 2014-02-26 | 浙江理工大学 | Preparation method of insect-protected starch slow release microspheres |
| CN106189497A (en) * | 2016-08-29 | 2016-12-07 | 苏州安洁科技股份有限公司 | A kind of spacetabs type fragrance water color ink |
| CN106491374B (en) * | 2016-12-06 | 2020-01-10 | 广州睿森生物科技有限公司 | Nepetalactone microcapsule, preparation method thereof and application of nepetalactone microcapsule in preparation of mosquito repellent product |
| CN106491374A (en) * | 2016-12-06 | 2017-03-15 | 广州睿森生物科技有限公司 | A kind of nepetalactone microcapsule and preparation method thereof with preparing the application in mosquito repellent product |
| CN106753898A (en) * | 2017-01-06 | 2017-05-31 | 南京福科帝生物科技有限公司 | A kind of odor prolongation clothes washing compositions of additives containing porous-starch and preparation method thereof |
| CN108354000A (en) * | 2018-04-19 | 2018-08-03 | 西安工程大学 | Fresh-keeping for fresh agricultural products slow, released microcapsule and preparation method thereof |
| CN111560771A (en) * | 2019-05-24 | 2020-08-21 | 安徽农业大学 | Embroidery anticorrosion and antioxidation method for three-dimensional pattern |
| CN110623076A (en) * | 2019-10-17 | 2019-12-31 | 湖北文理学院 | Instant walnut food containing rose essential oil and preparation method thereof |
| CN110982620A (en) * | 2019-11-26 | 2020-04-10 | 云南中烟工业有限责任公司 | Porous starch-loaded molecular capsule, and preparation method and application thereof |
| CN111820394A (en) * | 2020-09-21 | 2020-10-27 | 鲁东大学 | Preparation method of slow-release Chinese torreya shell essence |
| WO2022126913A1 (en) * | 2020-12-17 | 2022-06-23 | 天津春发生物科技集团有限公司 | Method for preparing liquid-type microcapsule product having flowability |
| CN114405423A (en) * | 2022-01-11 | 2022-04-29 | 广州乐居日化用品有限公司 | Porous chitosan microcapsule fragrance retaining bead and high-stability laundry gel bead |
| CN114711411A (en) * | 2022-03-31 | 2022-07-08 | 重庆小丸生物科技股份有限公司 | Self-dispersed oil microcapsule in water and preparation method thereof |
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Application publication date: 20120627 |