CN103046388A - Cool feeling microcapsule and preparation method thereof - Google Patents
Cool feeling microcapsule and preparation method thereof Download PDFInfo
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- CN103046388A CN103046388A CN2012105744362A CN201210574436A CN103046388A CN 103046388 A CN103046388 A CN 103046388A CN 2012105744362 A CN2012105744362 A CN 2012105744362A CN 201210574436 A CN201210574436 A CN 201210574436A CN 103046388 A CN103046388 A CN 103046388A
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- cool feeling
- diethylenetriamine
- paraphthaloyl chloride
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Abstract
The invention provides a cool feeling microcapsule and a preparation method thereof. The cool feeling microcapsule adopts one or several of menthol, menthone and eucalyptus as a core material, adopts paraphthaloyl chloride and diethylenetriamine as a wall material, and adopts interfacial polymerization to wrap the microcapsule in order to prepare the cool felling microcapsule. The preparation method for the cool feeling microcapsule has safe and simple technique and low cost; and the capsulation technique can improve the performance of cool feeling materials, can control the release speed thereof, and can widen the application range thereof.
Description
Technical field
What the present invention relates to is a kind of microcapsules and preparation method thereof, particularly relates to a kind of cool feeling microcapsules and preparation method thereof.
Background technology
A major function of clothes is the comfortableness of dress, and particularly in summer, the fabric of putting in order through the creeping chill agent can make human body produce nice and cool, comfortable sensation.Most creeping chill agent composition is take xylitol, menthol etc. as main, when being dissolved in the water, they can produce endothermic reaction, thereby temperature is reduced, when fabric contains the creeping chill material, the sweat gas in these creeping chill material absorbing bodies and producing endothermic reaction, thereby make skin produce cooling feeling, reduce skin surface temperature, but most creeping chill materials are volatile, run into photo-thermal and easily decompose, and affect its result of use.
Summary of the invention
Technical problem to be solved by this invention is: in the prior art, the creeping chill material is volatile, affects its result of use.
In order to solve this technical problem, the technical solution adopted in the present invention is:
The invention provides a kind of cool feeling microcapsules, these cool feeling microcapsules are take one or more of menthol, menthones, eucalyptus alcohol as core, and paraphthaloyl chloride and diethylenetriamine are the wall material.
The present invention also provides a kind of preparation method of above-mentioned cool feeling microcapsules, and concrete steps are:
(a) water preparation: POLYPROPYLENE GLYCOL 400, emulsifying agent and distilled water are added in the container successively, and the rear dropping pH adjusting agent that stirs is regulated pH to 8～9, saves backup,
As preferably: emulsifying agent is Tween-80,
As preferably: pH adjusting agent is triethanolamine,
As preferably: the mass ratio of POLYPROPYLENE GLYCOL 400, distilled water is 1:50～100, and the mass ratio of emulsifying agent, distilled water is 1:50～100;
(b) organic phase preparation: paraphthaloyl chloride and core material are dissolved in respectively in the cyclohexane,
As preferably: the mass ratio of paraphthaloyl chloride, core material is 1:3～5, and the cyclohexane solution concentration of paraphthaloyl chloride is 50g/L;
(c) emulsification: organic phase is scattered in aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min,
As preferably: the volume ratio of organic phase, water is 1:7～9;
(d) microencapsulation: under 30 ℃ of continuous stirring conditions, the cyclohexane solution of diethylenetriamine is at the uniform velocity added in the emulsifying systems, the constant until reaction of keeping system pH value finishes,
As preferably: the mass ratio of paraphthaloyl chloride, diethylenetriamine is 1:1～1.5, and the cyclohexane solution concentration of diethylenetriamine is 100g/L;
(e) discharging: filter, washing, dry, obtain the cool feeling microcapsules.
The invention has the beneficial effects as follows: the present invention prepares the creeping chill microcapsules with creeping chill material microencapsulations such as menthol, menthones, eucalyptus alcohol, avoids creeping chill material and external environment condition to react; Place the cool feeling microcapsules indoor summer, still can smell the distinctive the sort of aromatic odor of creeping chill material behind three wheat harvesting periods, illustrates that the creeping chill material is behind microencapsulation, can control its rate of release, play the effect of slowly-releasing, prolonged service time, enlarged the scope of application.Process safety of the present invention is simple, with low cost.
The specific embodiment
Embodiment 1
The water preparation: 6g POLYPROPYLENE GLYCOL 400,6g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 15g core material; The 25mL organic phase is scattered in the 175mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 50mL cyclohexane solution that is dissolved with the 5g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
The mensuration of core content in the microcapsules:
Microcapsules are placed flask, add the absolute ethyl alcohol of 5 times of amounts, and at 50 ℃ of lower backflow 3h, cooled and filtered is removed ethanol with filtrate 50 ℃ of lower fast decompression distillations, the remaining core quality of last weighing.
The mensuration of embedding rate:
Microcapsule embedded rate=(core content/core inventory in the microcapsules) * 100%
This product embedding rate 68.21%, the irregular spheroid of particle diameter 100～300nm, has good releasing effect, place the cool feeling microcapsules indoor summer, still can smell the distinctive the sort of aromatic odor of creeping chill material after 90 days, illustrate that the creeping chill material behind microencapsulation, has improved original performance, its effective release time was above 90 days.
Embodiment 2
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,4.5g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 20g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
This product embedding rate 72.6%(assay method such as embodiment 1), the irregular spheroid of particle diameter 100～250nm, has good releasing effect, place the cool feeling microcapsules indoor summer, still can smell the distinctive the sort of aromatic odor of creeping chill material after 110 days, illustrate that the creeping chill material behind microencapsulation, has improved original performance, its effective release time was above 110 days.
Embodiment 3
The water preparation: 3g POLYPROPYLENE GLYCOL 400,3g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 25g core material; The 25mL organic phase is scattered in the 225mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 75mL cyclohexane solution that is dissolved with the 7.5g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
This product embedding rate 66.33%(assay method such as embodiment 1), the irregular spheroid of particle diameter 100～270nm, has good releasing effect, place the cool feeling microcapsules indoor summer, still can smell the distinctive the sort of aromatic odor of creeping chill material after 100 days, illustrate that the creeping chill material behind microencapsulation, has improved original performance, its effective release time was above 100 days.
Comparative Examples 1
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,4.5gOP-10 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 20g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
This product embedding rate 70.26%(assay method such as embodiment 1), the irregular spheroid of particle diameter 150～750nm, compare with embodiment 2, only the emulsifier tween-80 with system changes OP-10 into, two kinds of product embedding rates that obtain are close, it is larger that particle diameter differs, and the particle diameter span is larger, so the present invention selects Tween-80 as the emulsifying agent of system.
Comparative Examples 2
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,4.5g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping NaOH aqueous solution that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 20g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
This product embedding rate 32.53%(assay method such as embodiment 1), compare with embodiment 2, only the pH adjusting agent triethanolamine with system changes the NaOH aqueous solution into, the average grain diameter of two kinds of products that obtain is close, it is larger that embedding rate differs, the embedding rate of Comparative Examples 2 is far below the embedding rate of embodiment 2, and this is because triethanolamine has certain solidification in system, so the present invention selects triethanolamine as the pH adjusting agent of system.
Comparative Examples 3
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,4.5g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 30g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
This product embedding rate 41.71%(assay method such as embodiment 1), compare with embodiment 2, increased the input amount of core material, the embedding rate of microcapsules diminishes, causing the waste of core material, is 1:3～5 so the present invention selects the mass ratio of phthalyl chloride, core material.
Comparative Examples 4
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,2g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 20g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
The irregular spheroid of this product cut size 200～800nm is compared with embodiment 2, has reduced the consumption of emulsifying agent, and it is large that the particle diameter span of microcapsules becomes, and is 1:50～100 so the present invention selects the mass ratio of Tween-80, distilled water.
Comparative Examples 5
The water preparation: 4.5g POLYPROPYLENE GLYCOL 400,7g Tween-80 and 300g distilled water are added in the container successively, and the rear dropping triethanolamine that stirs is regulated pH to 8～9, saves backup; Organic phase preparation: will be dissolved in respectively in the 100mL cyclohexane 5g paraphthaloyl chloride and 20g core material; The 25mL organic phase is scattered in the 200mL aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min; Under 30 ℃ of continuous stirring conditions, the 62.5mL cyclohexane solution that is dissolved with the 6.25g diethylenetriamine is at the uniform velocity added in the emulsifying systems, keeping system pH value is constant until the reaction end; Filter at last, wash, dry, obtain the cool feeling microcapsules.
The foam of system is too much during emulsification, can cause the cavity of microcapsules in the preparation process, is 1:50～100 so the present invention selects the mass ratio of Tween-80, distilled water.
Claims (8)
1. cool feeling microcapsules is characterized in that: described cool feeling microcapsules are take one or more of menthol, menthones, eucalyptus alcohol as core, and paraphthaloyl chloride and diethylenetriamine are the wall material.
2. the preparation method of cool feeling microcapsules as claimed in claim 1 is characterized in that: described preparation method is,
(a) water preparation: POLYPROPYLENE GLYCOL 400, emulsifying agent and distilled water are added in the container successively, and the rear dropping pH adjusting agent that stirs is regulated pH to 8～9, saves backup;
(b) organic phase preparation: be dissolved in respectively paraphthaloyl chloride and core material in the cyclohexane;
(c) emulsification: organic phase is scattered in aqueous phase, carries out emulsification, mixing speed 2000r/min, emulsification times 20min;
(d) microencapsulation: under 30 ℃ of continuous stirring conditions, the cyclohexane solution of diethylenetriamine is at the uniform velocity added in the emulsifying systems, the constant until reaction of keeping system pH value finishes;
(e) discharging: filter, washing, dry, obtain the cool feeling microcapsules.
3. the preparation method of cool feeling microcapsules as claimed in claim 2, it is characterized in that: the emulsifying agent described in the step (a) is Tween-80.
4. the preparation method of cool feeling microcapsules as claimed in claim 2, it is characterized in that: the pH adjusting agent described in the step (a) is triethanolamine.
5. the preparation method of cool feeling microcapsules as claimed in claim 2, it is characterized in that: the mass ratio of the POLYPROPYLENE GLYCOL 400 described in the step (a), distilled water is 1:50～100, the mass ratio of emulsifying agent, distilled water is 1:50～100.
6. the preparation method of cool feeling microcapsules as claimed in claim 2, it is characterized in that: the mass ratio of the paraphthaloyl chloride described in the step (b), core material is 1:3～5, the cyclohexane solution concentration of paraphthaloyl chloride is 50g/L.
7. the preparation method of cool feeling microcapsules as claimed in claim 2, it is characterized in that: the volume ratio of the organic phase described in the step (c), water is 1:7～9.
8. the preparation method of cool feeling microcapsules claimed in claim 2, it is characterized in that: the mass ratio of the paraphthaloyl chloride described in the step (d), diethylenetriamine is 1:1～1.5, the cyclohexane solution concentration of diethylenetriamine is 100g/L.
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| CN201210574436.2A CN103046388B (en) | 2012-12-25 | 2012-12-25 | Cool feeling microcapsule and preparation method thereof |
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Cited By (7)
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| CN104194931A (en) * | 2014-07-16 | 2014-12-10 | 广西中烟工业有限责任公司 | Menthol-loaded porous polymer microsphere tobacco spice slow-release material 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 |
| CN107675560A (en) * | 2017-05-24 | 2018-02-09 | 湖北中烟工业有限责任公司 | Cigarette aluminium-foil paper preparation method with slow controlled release cool feeling essence |
| CN108066165A (en) * | 2017-12-22 | 2018-05-25 | 江山 | A kind of toothpaste particle and preparation method thereof and the application in toothpaste |
| CN111513389A (en) * | 2020-05-05 | 2020-08-11 | 南通大学 | Breathable and comfortable cool mask and preparation method thereof |
| CN111560258A (en) * | 2020-05-27 | 2020-08-21 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive color developing liquid crystal microcapsule and preparation method thereof |
| CN115627641A (en) * | 2022-09-26 | 2023-01-20 | 黛思(常州)无纺布有限公司 | Lasting mask cool feeling agent and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194931A (en) * | 2014-07-16 | 2014-12-10 | 广西中烟工业有限责任公司 | Menthol-loaded porous polymer microsphere tobacco spice slow-release material 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 |
| CN107675560A (en) * | 2017-05-24 | 2018-02-09 | 湖北中烟工业有限责任公司 | Cigarette aluminium-foil paper preparation method with slow controlled release cool feeling essence |
| CN108066165A (en) * | 2017-12-22 | 2018-05-25 | 江山 | A kind of toothpaste particle and preparation method thereof and the application in toothpaste |
| CN111513389A (en) * | 2020-05-05 | 2020-08-11 | 南通大学 | Breathable and comfortable cool mask and preparation method thereof |
| CN111560258A (en) * | 2020-05-27 | 2020-08-21 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive color developing liquid crystal microcapsule and preparation method thereof |
| CN112175632A (en) * | 2020-05-27 | 2021-01-05 | 江苏集萃智能液晶科技有限公司 | Temperature-sensitive color developing liquid crystal microcapsule and preparation method thereof |
| CN115627641A (en) * | 2022-09-26 | 2023-01-20 | 黛思(常州)无纺布有限公司 | Lasting mask cool feeling agent and preparation method thereof |
| CN115627641B (en) * | 2022-09-26 | 2024-02-13 | 黛思(常州)无纺布有限公司 | Lasting mask cool feeling agent and preparation method thereof |
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| CN103046388B (en) | 2014-10-15 |
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