CN105124517A - Preparation method of cooling compound microcapsule - Google Patents
Preparation method of cooling compound microcapsule Download PDFInfo
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- CN105124517A CN105124517A CN201510574670.9A CN201510574670A CN105124517A CN 105124517 A CN105124517 A CN 105124517A CN 201510574670 A CN201510574670 A CN 201510574670A CN 105124517 A CN105124517 A CN 105124517A
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Abstract
The invention relates to a preparation method of a cooling compound microcapsule. The preparation method comprises the following steps: the step (1): mixing propylene glycol, tween-80, nonyl phenol polyoxyethylene ether and span-60, and obtaining a carrier solution; the step (2): adding a cooling compound to the carrier solution to be dissolved, and uniformly stirring and mixing the carrier solution and the cooling compound so as to obtain a core material; and the step (3), adding the core material to a cyclodextrin solution, performing vibration and clathration for some time by using ultrasonic waves so as to obtain products, and drying the products. According to the microcapsule prepared by the method disclosed by the invention, the entrapping rate can reach more than 75%. The method has the advantages that the method is simple and environmental-friendly, and effective components in the cooling compound are not liable to volatilize.
Description
Technical field
The invention belongs to coolant agent application, be specifically related to a kind of preparation method of coolant agent microcapsules.
Background technology
Coolant agent is the general name of a class material that can produce cooling effect, and it can, to the temperature sensor generation effect of human body, allow people produce cool feeling by cold sensor.Modal natural coolant agent is levorotatory menthol, but due to its cool feeling action time not long, and can bitter taste be produced when addition is larger, therefore synthesize coolant agent and be developed gradually.At present synthesis coolant agent common on the market has WS-3(N-ethyl-to menthyl-3-formamide), WS-23(2-isopropyl-N, 2,3-trimethylbutyramide), WS-5(acetic acid (N-ethyl-to menthyl-3-carboxylic acid amides) ethyl ester) etc., it is active that they have high cool taste mostly, and there is no the side effects such as calcination, numbness and stimulation, be widely used in the product of food, daily use chemicals, medicine and other fields.
Microcapsules technology is a kind of filmogen the technology of solid or the coated formation fine particle of liquid, and microcapsules are made up of core and wall material, and cyclodextrin is then a kind of more common microcapsule wall material.The kind of cyclodextrin is a lot, common are alpha-cyclodextrin, beta-schardinger dextrin-, gamma-cyclodextrin, HP-β-CD etc.Cyclodextrin molecular is inner based on C-H bond and ehter bond, has hydrophobicity.Outside is then based on hydroxyl, has hydrophily.Oil loving material can be combined with cyclodextrin inner hydrophobic parts, and cyclodextrin encapsulated, can the solubility property of this oleophilic substance of improvement in various degree.In addition due to after oleophilic substance inclusion enters cyclodextrin, cyclodextrin plays a protective role to guest molecule, in external condition as solvent, pH, temperature, oxygen etc., is not easy, to it, effects such as oxydrolysis occur, thus maintains the stability of inner guest molecule.The material of liquid can make its powdered after cyclodextrin encapsulated, makes granule or powder etc., and effectively prevents effumability composition from volatilizing, and reduces the stimulation of medicine and has slow releasing function etc.
No matter be levorotatory menthol, or coolant agent WS-23, WS-3, WS-5, they in aqueous or insoluble, or dissolubility very little, and the time that their cool feeling degree continues is all relatively short.And utilize cyclodextrin to wrap up after above-mentioned coolant agent makes microcapsules, can highly effective solution they use in food, medicine etc. in disperse uneven problem, cool taste rate of release is too fast, and cool feeling degree can be held time the problem such as long.
Existing coolant agent microcapsules patent mainly uses the macromolecular material of two kinds of oppositely chargeds as composite sac material, under certain condition by coolant agent molecule parcel wherein, and cross-linked cohesion encystation.As " a kind of preparation methods of amide of mint microcapsules " patent that application number is 201010608333.4, disclose and use water soluble protein and natural gum as wall material, wrap up amide of mint molecule.The weak point of this method is, manufacture craft is comparatively complicated, and CCP is more, and the chemical reagent used has a small amount of toxicity." a kind of preparation method of menthol microcapsules " patent of application number 201010270636.X, discloses and uses shitosan to be wall material, add modified starch and be cross-linked the method preparing menthol microcapsules.The weak point of this method is, the microcapsules aqueous solution is difficult to filter, and spray-dired method must be used to process.
Summary of the invention
For Problems existing in the practical application of coolant agent in food and medicine etc., the invention provides a kind of preparation method of coolant agent microcapsules.The microcapsules be prepared from have not volatile, cool feeling degree is gentle and the feature such as slowly-releasing.
The present invention is achieved through the following technical solutions:
A preparation method for coolant agent microcapsules, comprises the following steps:
Step (1): by propane diols, Tween-80, NPE, Arlacel-60 mixing, obtain carrier solvent;
Step (2): coolant agent is joined in above-mentioned carrier solvent and dissolves, be core after being uniformly mixed;
Step (3): added in cyclodextrin solution by above-mentioned core, and obtain product after using ultrasonic oscillation inclusion a period of time, by after described product drying and get final product.
Preferably, the mass ratio of described propane diols, Tween-80, NPE, Arlacel-60 is 5:3:1:1;
Preferably, the mass ratio of described coolant agent and described carrier solvent controls at 1:5-1:8; Preferred further, described coolant agent is one or several the mixing in levorotatory menthol, WS-23, WS-3, WS-5.
Preferably, described cyclodextrin is the mixing of one or more in alpha-cyclodextrin, methyl-B-cyclodextrin, 2,6-DM-β-CDs, HP-β-CD.
Preferably, described ultrasonic oscillation inclusion instrument is numerical control supersonic concussion instrument; Preferred further, described supersonic frequency controls at 25-40KHZ, and inclusion reaction temperature controls at 50-80 DEG C, and inclusion reaction time controling is at 0.5-5h.
Preferably, the described drying mode by described product drying is vacuum drying; Preferred further, described vacuum drying temperature is 25-50 DEG C.
Beneficial effect of the present invention:
The advantages such as microcapsule embedded rate prepared by the inventive method can reach more than 75%, and it is simple to have method, environmental protection, safety nuisance free, and coolant agent active ingredient is not volatile, the gentle and slowly-releasing of cool feeling degree.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): levorotatory menthol is joined in above-mentioned carrier solvent and dissolves, the mass ratio of levorotatory menthol and described carrier solvent is 1:5, is core after being uniformly mixed;
Step (3): being added by above-mentioned core in methyl-B-cyclodextrin solution and to use ultrasonic oscillation inclusion 0.5h, supersonic frequency is 25KHZ, and inclusion reaction temperature is 50 DEG C, by products therefrom 25 DEG C of vacuum drying and get final product.
embodiment 2
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1), the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mix, and obtain carrier solvent;
Step (2): coolant agent WS-3 is joined in above-mentioned carrier solvent and dissolves, the mass ratio of WS-3 and described carrier solvent is 1:8, is core after being uniformly mixed; ;
Step (3): being added by above-mentioned core in methyl-B-cyclodextrin solution and to use ultrasonic oscillation inclusion 5h, supersonic frequency is 40KHZ, and inclusion reaction temperature is 80 DEG C, by products therefrom 50 DEG C of vacuum drying and get final product.
embodiment 3
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): coolant agent WS-5 is joined in above-mentioned carrier solvent and dissolves, the mass ratio of WS-5 and described carrier solvent is 1:5, is core after being uniformly mixed; ;
Step (3): being added by above-mentioned core in alpha-cyclodextrin solution and to use ultrasonic oscillation inclusion 3h, supersonic frequency is 30KHZ, and inclusion reaction temperature is 65 DEG C, by products therefrom 45 DEG C of vacuum drying and get final product.
embodiment 4
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): coolant agent WS-23 is joined in above-mentioned carrier solvent and dissolves, the mass ratio of WS-23 and described carrier solvent is 1:5, is core after being uniformly mixed; ;
Step (3): being added by above-mentioned core in 2,6-DM-β-CD solution and to use ultrasonic oscillation inclusion 1h, supersonic frequency is 35KHZ, and inclusion reaction temperature is 60 DEG C, by products therefrom 40 DEG C of vacuum drying and get final product.
embodiment 5
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): levorotatory menthol, WS-3 are joined in above-mentioned carrier solvent and dissolved, and the mass ratio of levorotatory menthol, WS-3 and described carrier solvent is 1:6, is core after being uniformly mixed;
Step (3): being added by above-mentioned core in the mixed solution of methyl-B-cyclodextrin and HP-β-CD and to use ultrasonic oscillation inclusion 1.5h, supersonic frequency is 29KHZ, and inclusion reaction temperature is 65 DEG C, by products therefrom 45 DEG C of vacuum drying and get final product.
embodiment 6
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): coolant agent WS-3, WS-23, WS-5 are joined in above-mentioned carrier solvent and dissolves, the mass ratio of WS-3, WS-23, WS-5 and described carrier solvent is 1:5, is core after being uniformly mixed;
Step (3): above-mentioned core is added methyl-B-cyclodextrin, HP-β-CD, 2, ultrasonic oscillation inclusion 2h is used in the mixed solution of 6-DM-β-CD, supersonic frequency is 35KHZ, and inclusion reaction temperature is 75 DEG C, by products therefrom 50 DEG C of vacuum drying and get final product.
embodiment 7
The present embodiment relates to a kind of preparation method of coolant agent microcapsules, comprises the following steps:
Step (1): the ratio being 5:3:1:1 according to mass ratio by propane diols, Tween-80, NPE, Arlacel-60 mixes, obtains carrier solvent;
Step (2): levorotatory menthol, WS-3, WS-23, WS-5 are joined in above-mentioned carrier solvent and dissolve, the mass ratio of levorotatory menthol, WS-3, WS-23, WS-5 and described carrier solvent is 1:8, is core after being uniformly mixed;
Step (3): above-mentioned core is added alpha-cyclodextrin, methyl-B-cyclodextrin, 2, ultrasonic oscillation inclusion 3.5h is used in the mixed solution of 6-DM-β-CD, HP-β-CD, supersonic frequency is 35KHZ, inclusion reaction temperature is 70 DEG C, by products therefrom 45 DEG C of vacuum drying and get final product.
Claims (9)
1. a preparation method for coolant agent microcapsules, is characterized in that, comprises the following steps:
Step (1): by propane diols, Tween-80, NPE, Arlacel-60 mixing, obtain carrier solvent;
Step (2): coolant agent is joined in above-mentioned carrier solvent and dissolves, be core after being uniformly mixed;
Step (3): added in cyclodextrin solution by above-mentioned core, and obtain product after using ultrasonic oscillation inclusion a period of time, by after described product drying and get final product.
2. the preparation method of coolant agent microcapsules according to claim 1, is characterized in that, in described step (1), in described carrier solvent, the mass ratio of propane diols, Tween-80, NPE, Arlacel-60 is 5:3:1:1.
3. the preparation method of coolant agent microcapsules according to claim 1, is characterized in that, in described step (2), described coolant agent is the mixing of one or more of levorotatory menthol, WS-23, WS-3, WS-5.
4. the preparation method of coolant agent microcapsules according to claim 1, is characterized in that, in described step (2), the mass ratio of described coolant agent and described carrier solvent controls at 1:5-1:8.
5. the preparation method of coolant agent microcapsules according to claim 1, is characterized in that, in described step (3), uses the instrument of ultrasonic oscillation inclusion to shake instrument for numerical control supersonic.
6. the preparation method of coolant agent microcapsules according to claim 5, is characterized in that, in described step (3), the FREQUENCY CONTROL of described supersonic oscillations instrument is at 25-40KHZ, and inclusion reaction temperature controls as 50-80 DEG C, and inclusion time controling is at 0.5-5h.
7. the preparation method of coolant agent microcapsules according to claim 1, it is characterized in that, in described step (3), described cyclodextrin is the mixing of one or more in alpha-cyclodextrin, methyl-B-cyclodextrin, 2,6-DM-β-CDs, HP-β-CD.
8. the preparation method of coolant agent microcapsules according to claim 1, is characterized in that, in described step (3), drying mode adopts vacuum drying.
9. the preparation method of coolant agent microcapsules according to claim 8, is characterized in that, in described step (3), vacuum drying temperature controls at 25-50 DEG C.
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Cited By (8)
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| CN105832580A (en) * | 2016-05-10 | 2016-08-10 | 安徽爱迪香料股份有限公司 | Preparing method for functional shampoo containing essential oil microcapsules |
| CN107751522A (en) * | 2017-11-09 | 2018-03-06 | 安徽爱迪香料股份有限公司 | A kind of overlength cool feeling duration pressed candy and preparation method thereof |
| CN108634294A (en) * | 2018-04-20 | 2018-10-12 | 珠海首力企业有限公司 | A kind of surely effect coolant agent and preparation process |
| CN109452523A (en) * | 2018-12-07 | 2019-03-12 | 昆山亚香香料股份有限公司 | Drink coolant agent component and its method for making |
| CN109463510A (en) * | 2018-12-25 | 2019-03-15 | 安徽爱迪香料股份有限公司 | A method of pressed candy is prepared using the long-acting coolant agent of eutectic |
| CN109576099A (en) * | 2018-12-07 | 2019-04-05 | 昆山亚香香料股份有限公司 | For the coolant agent component in beer and its it is made into method |
| CN109593628A (en) * | 2018-12-07 | 2019-04-09 | 昆山亚香香料股份有限公司 | Enhance the cool taste component formula and preparation method thereof of the cool degree of drinks |
| CN113142549A (en) * | 2021-04-19 | 2021-07-23 | 良品铺子股份有限公司 | Composite microcapsule type fat substitute and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105832580A (en) * | 2016-05-10 | 2016-08-10 | 安徽爱迪香料股份有限公司 | Preparing method for functional shampoo containing essential oil microcapsules |
| CN107751522A (en) * | 2017-11-09 | 2018-03-06 | 安徽爱迪香料股份有限公司 | A kind of overlength cool feeling duration pressed candy and preparation method thereof |
| CN108634294A (en) * | 2018-04-20 | 2018-10-12 | 珠海首力企业有限公司 | A kind of surely effect coolant agent and preparation process |
| CN108634294B (en) * | 2018-04-20 | 2022-05-10 | 珠海首力企业有限公司 | Stable-effect cooling agent and preparation process thereof |
| CN109452523A (en) * | 2018-12-07 | 2019-03-12 | 昆山亚香香料股份有限公司 | Drink coolant agent component and its method for making |
| CN109576099A (en) * | 2018-12-07 | 2019-04-05 | 昆山亚香香料股份有限公司 | For the coolant agent component in beer and its it is made into method |
| CN109593628A (en) * | 2018-12-07 | 2019-04-09 | 昆山亚香香料股份有限公司 | Enhance the cool taste component formula and preparation method thereof of the cool degree of drinks |
| CN109463510A (en) * | 2018-12-25 | 2019-03-15 | 安徽爱迪香料股份有限公司 | A method of pressed candy is prepared using the long-acting coolant agent of eutectic |
| CN113142549A (en) * | 2021-04-19 | 2021-07-23 | 良品铺子股份有限公司 | Composite microcapsule type fat substitute and preparation method thereof |
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Application publication date: 20151209 |