CN102068947A - Preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules - Google Patents
Preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules Download PDFInfo
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- CN102068947A CN102068947A CN 201010608333 CN201010608333A CN102068947A CN 102068947 A CN102068947 A CN 102068947A CN 201010608333 CN201010608333 CN 201010608333 CN 201010608333 A CN201010608333 A CN 201010608333A CN 102068947 A CN102068947 A CN 102068947A
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Abstract
The invention provides a preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules. The preparation method comprises the following steps: (1) stirring and mixing N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide solution, water-soluble protein aqueous solution and gum aqueous solution and adding hydrochloric acid or acetic acid to regulate the pH value of the solution to be 3.5-4.5; and (2) adding glutaradehyde solution, stirring and mixing the mixture to obtain wet microcapsules, then filtering the wet microcapsules and carrying out vacuum freeze drying, thus obtaining the powder-like N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules. The preparation method has the following beneficial effects: N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide is prepared into microcapsules; the existential state, weight and volume of the N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide are improved so that the N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide is suitable for versatile processing environments; the N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide is avoided from reacting with the external environment so that the release speed can be controlled and the duration of playing a role of slow release is longer; and toxicity is reduced and the color is maintained. The preparation method has the advantages of simple process, safe operation and easy control, and the formed microcapsules have compact wall membranes and good release performance.
Description
Technical field
The present invention relates to the preparation method of amide of mint microcapsules.
Background technology
Amide of mint of the present invention chemistry N-ethy-2-isopropyl-5-methylcyclohexanecarboxamide by name (N-ethyl-2-different-propyl group-5-methyl-cyclohexyl alkane acid amides), be a kind of white crystalline powder, be slightly soluble in water, be dissolved in most of organic solvents, slight camphor flavor is arranged, be mainly used in as the cool agent of the system in medicine, MC, the candy, and, have excellent anthelminthic effect and cooling effect in the pest repellant field.
Improve described amide of mint existence,, avoid amide of mint and external environment condition to react to be suitable for changeable processing environment, so that the control rate of release, and can play the effect of slowly-releasing, reduce toxicity, keep color and luster, can make the wider of amide of mint use.
With the amide of mint microencapsulation, be method commonly used at present, the amide of mint behind the microencapsulation can be widely used in a plurality of fields such as medicine, health care of food, agricultural chemicals, essence and flavoring agent.
The common method of microencapsulation has reached kind more than 200 at present, yet these methods respectively have pluses and minuses, consider the particularity of amide of mint, and present technology seldom has can be directly used in the amide of mint microencapsulation, does not also have relevant document and patent.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of amide of mint microcapsules is to overcome the defective that prior art exists.
Method of the present invention comprises as step as follows:
(1) amide of mint solution and the water soluble protein aqueous solution, the gummy aqueous solution are stirred mixed in 30～60 minutes, the adding weight concentration is that 5～10% hydrochloric acid or weight concentration are 5～10% acetic acid regulator solution pH to 3.5～4.5;
The weight of amide of mint: the weight of water-solubility protein=1: 10～10: 1;
Preferably, the weight of amide of mint: the weight of water-solubility protein=1: 1～2;
Natural gum: the weight of water-solubility protein=1: 10～10: 1;
Preferably, natural gum: the weight of water-solubility protein=0.3～2: 1;
Described amide of mint solution is the mixture of amide of mint and propyl lactate, ethyl acetate, propyl acetate or carrene, and the weight concentration of amide of mint is 1～5%;
Described water soluble protein is selected from gelatin, soybean protein isolate or wheat water-solubility protein, and the weight concentration of the water soluble protein aqueous solution is 0.5%～5%;
Described natural gum is selected from Arabic gum, bassora gum or melamine resin; The weight concentration of the natural gum aqueous solution is 0.5%～5%;
(2) add glutaraldehyde solution, stir mixing in 30～60 minutes, obtain wet microcapsules, filter then, vacuum freeze drying promptly obtains pulverous amide of mint microcapsules;
The weight of glutaraldehyde: the weight of water-solubility protein=1: 20～1: 5;
Preferably, the weight of glutaraldehyde: the weight of water-solubility protein=1: 1.5～6;
The weight concentration of glutaraldehyde solution is preferably 0.1～5%, and excessive concentration can cause the microcapsules bonding;
Tool of the present invention can make the wider of amide of mint use with the amide of mint microencapsulation, improves its existence, weight and volume; Be suitable for changeable processing environment; Avoid amide of mint and external environment condition to react; Can control rate of release, the acting duration that plays slowly-releasing is longer; Reduce toxicity; Keep color and luster.Behind the amide of mint microencapsulation, can in a plurality of fields such as medicine, health care of food, agricultural chemicals, essence and flavoring agent, be applied, and developed.Technology of the present invention is simple, and handling safety is easy to control, the preparation method of the amide of mint microcapsules that the microcapsule wall film densification of formation and release performance are good.
Description of drawings
Fig. 1 is the exterior appearance of the observed microcapsule product of Electronic Speculum SEM.
The specific embodiment
Embodiment 1
Get gelatin 0.3g, dissolve, obtain weight concentration and be 2% aqueous gelatin solution with the ionized water of 40 ℃ of 14.7g, standby;
Get Arabic gum 0.6g, dissolve, obtain concentration and be 2% the Arabic gum aqueous solution with the ionized water of 40 ℃ of 29.4g, standby;
Take by weighing amide of mint 0.3g, dissolve, obtain concentration and be 3% amide of mint solution with the 9.7g propyl lactate;
Pour amide of mint solution into gelatin solution, add the Arabic gum aqueous solution, stirred 30 minutes, the adding weight concentration is that 10% hydrochloric acid makes pH to 4.5;
The adding weight concentration is 5% glutaraldehyde solution 4g, stirs 30 minutes, obtains wet microcapsules;
Use sand core funnel that microcapsule solution is carried out suction filtration, place vacuum freeze drier again, 10Pa vacuum and-5 ℃ of dryings promptly obtain pulverous amide of mint microcapsules.
Fig. 1 has provided the exterior appearance that adopts the observed microcapsule product of scanning electron microscope sem.Microcapsule granule is even as seen from Figure 1, outward appearance slyness, the densification of wall film; By the mensuration of laser particle analyzer, the particle diameter that obtains microcapsules is at 5～20 μ m; According to infrared analysis, determine that the wall material has coated core, its clad ratio is 84.6%; Through check, the microcapsule product that obtains is white in color, and has no irritating odor.
Embodiment 2
Get soybean protein isolate 0.6g, water dissolves, and obtains weight concentration and be 5% the soybean protein isolate aqueous solution, and is standby;
Get bassora gum 0.9g, water dissolves, and obtains weight concentration and be 5% the bassora gum aqueous solution, and is standby;
Take by weighing amide of mint 0.6g, dissolve, obtain weight concentration and be 1% amide of mint solution with 59.4g ethyl acetate;
Pour amide of mint solution into the soybean protein isolate aqueous solution, add the bassora gum aqueous solution, stirred 60 minutes, the adding weight concentration is that 5% acetic acid makes pH to 3.5;
The adding weight concentration is 1% glutaraldehyde solution 10g, stirs 60 minutes, obtains wet microcapsules; Use sand core funnel that microcapsule solution is carried out suction filtration, place vacuum freeze drier again, 10Pa vacuum and-5 ℃ of dryings promptly obtain pulverous amide of mint microcapsules.
By the mensuration of laser particle analyzer, the particle diameter that obtains microcapsules is at 10～40 μ m; According to infrared analysis, determine that the wall material has coated core, its clad ratio is 72.3%; Through check, the microcapsule product that obtains is white in color, and has no irritating odor.
Embodiment 3
Get wheat water-solubility protein 0.9g, water dissolves, and obtains weight concentration and be 1% the wheat water-solubility protein aqueous solution, and is standby;
Get melamine resin 0.3g, water dissolves, and obtains weight concentration and be 1% the melamine resin aqueous solution, and is standby;
Take by weighing amide of mint 0.9g, dissolve, obtain weight concentration and be 2% amide of mint solution with 44.1g ethyl acetate;
Pour amide of mint solution into the wheat water-solubility protein aqueous solution, add the melamine resin aqueous solution, stirred 40 minutes, the adding weight concentration is that 5% acetic acid makes pH to 4.0;
The adding weight concentration is 5% glutaraldehyde solution 8g, stirs 40 minutes, obtains wet microcapsules; Use sand core funnel that microcapsule solution is carried out suction filtration, place vacuum freeze drier again, 10Pa vacuum and?-5 ℃ of dryings promptly obtain pulverous amide of mint microcapsules.
Recording its clad ratio is 75.8%; By the mensuration of laser particle analyzer, the particle diameter that obtains microcapsules is at 15～40 μ m; Through check, the microcapsule product that obtains is white in color, and has no irritating odor.
Claims (10)
1. the preparation method of amide of mint microcapsules is characterized in that, comprises as step as follows:
(1) amide of mint solution and the water soluble protein aqueous solution, the gummy aqueous solution are mixed, add hydrochloric acid or acetic acid regulator solution pH to 3.5～4.5;
(2) add glutaraldehyde solution, mix, obtain wet microcapsules, filter then, vacuum freeze drying promptly obtains pulverous amide of mint microcapsules.
2. method according to claim 1 is characterized in that, the weight of amide of mint: the weight of water-solubility protein=1: 10～10: 1.
3. method according to claim 1 is characterized in that, the weight of amide of mint: the weight of water-solubility protein=1: 1～3.
4. method according to claim 1 is characterized in that natural gum: the weight of water-solubility protein=1: 10～10: 1.
5. method according to claim 1 is characterized in that natural gum: the weight of water-solubility protein=0.3～2: 1.
6. method according to claim 1 is characterized in that, described amide of mint solution is the mixture of amide of mint and propyl lactate, ethyl acetate, propyl acetate or carrene, and the weight concentration of amide of mint is 1～5%.
7. method according to claim 1 is characterized in that described water soluble protein is selected from gelatin, soybean protein isolate or wheat water-solubility protein, and the weight concentration of the water soluble protein aqueous solution is 0.5%～5%.
8. method according to claim 1 is characterized in that described natural gum is selected from Arabic gum, bassora gum or melamine resin; The weight concentration of the natural gum aqueous solution is 0.5%～5%.
9. method according to claim 1 is characterized in that, the weight of glutaraldehyde: the weight of water-solubility protein=1: 20～1: 5.
10. method according to claim 1 is characterized in that, the weight of glutaraldehyde: the weight of water-solubility protein=1: 1.5～6.
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| CN 201010608333 CN102068947A (en) | 2010-12-28 | 2010-12-28 | Preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250403A (en) * | 2011-06-27 | 2011-11-23 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN103340196A (en) * | 2013-07-16 | 2013-10-09 | 东北林业大学 | Leaf alcohol microcapsule and preparation method thereof |
| CN104988742A (en) * | 2015-06-11 | 2015-10-21 | 江苏阳光股份有限公司 | Cold-feeling easy-care treating method of cotton shirt |
| CN105413597A (en) * | 2015-12-14 | 2016-03-23 | 安徽丰乐香料有限责任公司 | Preparation method of peppermint oil microcapsules |
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| CN1251388A (en) * | 1999-03-22 | 2000-04-26 | 山东农业大学 | Micro-capsule peridium growth regulator |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250403A (en) * | 2011-06-27 | 2011-11-23 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN102250403B (en) * | 2011-06-27 | 2012-12-19 | 上海工程技术大学 | Multifunctional agricultural thin film and preparation method thereof |
| CN103340196A (en) * | 2013-07-16 | 2013-10-09 | 东北林业大学 | Leaf alcohol microcapsule and preparation method thereof |
| CN104988742A (en) * | 2015-06-11 | 2015-10-21 | 江苏阳光股份有限公司 | Cold-feeling easy-care treating method of cotton shirt |
| CN104988742B (en) * | 2015-06-11 | 2017-06-13 | 江苏阳光股份有限公司 | A kind of cool feeling no-iron treatment method of cotton shirt |
| CN105413597A (en) * | 2015-12-14 | 2016-03-23 | 安徽丰乐香料有限责任公司 | Preparation method of peppermint oil microcapsules |
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Application publication date: 20110525 |