CN108993332B - Preparation method of heat-resistant essence microcapsule - Google Patents
Preparation method of heat-resistant essence microcapsule Download PDFInfo
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- CN108993332B CN108993332B CN201810845871.1A CN201810845871A CN108993332B CN 108993332 B CN108993332 B CN 108993332B CN 201810845871 A CN201810845871 A CN 201810845871A CN 108993332 B CN108993332 B CN 108993332B
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/046—Making microcapsules or microballoons by physical processes, e.g. drying, spraying combined with gelification or coagulation
Abstract
A preparation method of a heat-resistant essence microcapsule comprises the following steps: (1) mixing silicate ester, alkali and absolute ethyl alcohol, and then dropwise adding the mixture into a first ethanol aqueous solution at a certain temperatureCarrying out hydrolysis-polycondensation reaction to obtain SiO2Sol; (2) adding essence into a solvent, uniformly mixing, then adding a surfactant, and regulating with an alkali solution to obtain an alkaline system; (3) adding the alkaline system obtained in the step (2) into the SiO obtained in the step (1)2Mixing the sol for a period of time, washing and separating the obtained suspension liquid with water for multiple times until the suspension liquid is neutral, and obtaining a solid; (4) and (4) washing and separating the solid obtained in the step (3) for multiple times by using a second ethanol aqueous solution, and drying the obtained solid in vacuum to obtain the heat-resistant essence microcapsule. The preparation method of the essence microcapsule is simple, and the prepared essence microcapsule has high essence utilization rate. The essence microcapsule prepared by the preparation method has stable fragrance and lasting fragrance at the temperature of about 90 ℃.
Description
Technical Field
The invention belongs to the technical field of slow-release essence preparation, and particularly relates to a sol-gel preparation method of a heat-resistant essence microcapsule.
Background
Essence as a substance with strong volatility can be quickly perceived by human body, but the persistence is generally poor. The sustained and controlled release technology is a substance controlled release technology, and the target substance is slowly or controllably released in a release medium by carrying out certain treatment on the target substance or depending on certain special properties of auxiliary materials. By carrying out sustained and controlled release treatment on the essence, the aim of prolonging the aroma release time can be achieved, and other auxiliary aims such as improving the thermal stability of the essence can be achieved. The microcapsule is a common typical storage type slow controlled release system of perfume essence, which is composed of a capsule wall and an inner core, and usually some natural or synthetic high molecular materials are used as the capsule wall, such as natural gum arabic, gelatin, chitosan, beta-cyclodextrin and cellulose. The microcapsule essence has poor heat resistance.
Silicon material is also one of the more common load bearing materials. The silicon material has good biocompatibility and structural stability, and due to the development of a surfactant template method in recent years, the preparation of the silicon-based mesoporous material is more convenient, and the aperture and the shape of the silicon-based mesoporous material are adjustable, so that the silicon-based mesoporous material is one of the best sustained and controlled release carriers.
The silicon material is used for preparing the wall material of the essence microcapsule for the first time.
Disclosure of Invention
The invention aims to provide a method for preparing essence microcapsules by sol-gel and application thereof, aiming at the defect of poor heat resistance of the essence microcapsules in the prior art.
The invention takes Tetraethoxysilane (TEOS) as a wall material precursor, essence as a core material, 2-methoxyethanol and deionized water as a cosolvent system, alkali as a catalyst, and hexadecyltrimethylammonium bromide and dodecyltrimethylammonium bromide as mixed template agents, prepares the heat-resistant mesoporous silica essence microcapsule at room temperature by a sol-gel method, and judges the release temperature and the release amount of the embedded essence and spice by thermogravimetric analysis. The preparation method provided by the invention is simple in preparation process, and the prepared essence microcapsule is high in thermal stability and utilization rate of essence.
The purpose of the invention is realized by the following technical scheme.
The invention discloses a preparation method of a heat-resistant essence microcapsule, which comprises the following steps:
(1) silicon is mixedAcid ester, alkali and absolute ethyl alcohol are mixed and then are dripped into the first ethanol water solution to carry out hydrolysis-polycondensation reaction at a certain temperature to prepare SiO2Sol;
(2) adding essence into a solvent, uniformly mixing, then adding a surfactant, and regulating with an alkali solution to obtain an alkaline system;
the steps (1) and (2) are not sequenced;
(3) adding the alkaline system obtained in the step (2) into the SiO obtained in the step (1)2Mixing the sol for a period of time, washing and separating the obtained suspension liquid with water for multiple times until the suspension liquid is neutral, and obtaining a solid;
(4) and (4) washing and separating the solid obtained in the step (3) for multiple times by using a second ethanol aqueous solution, and drying the obtained solid in vacuum to obtain the heat-resistant essence microcapsule.
Preferably, the silicate in the step (1) is ethyl orthosilicate, and the first ethanol aqueous solution is 50 wt% ethanol aqueous solution; the hydrolysis-polycondensation reaction temperature is 60-80 ℃.
Preferably, the essence in the step (2) is one or more of menthol, lemon essence, sweet orange essence, lily essence or rose essence, and the solvent is 2-methoxy ethanol aqueous solution; the surfactant is a mixture of hexadecyl trimethyl ammonium bromide and dodecyl trimethyl ammonium bromide; the alkalinity is that the pH value is 11-13.
Preferably, the second ethanol aqueous solution in the step (4) is 75 wt% ethanol aqueous solution; the temperature of the vacuum drying is 40-50 ℃, and the time is 24-48 h.
The invention also discloses application of the heat-resistant essence microcapsule prepared by the preparation method in tobacco products.
The invention relates to a specific preparation method of a heat-resistant essence microcapsule, which comprises the following specific steps:
(1) mixing 50mL of ethyl orthosilicate, 30mL of 0.1mol/L sodium hydroxide and 30mL of absolute ethyl alcohol, stirring at room temperature, then dropwise adding 30mL of 50 wt% ethanol aqueous solution for hydrolysis-polycondensation reaction, heating to 70 ℃ after 1h of reaction, and polymerizing for 2h at constant temperature to obtain SiO2Sol;
(2) adding 1-2 g of essence (one of menthol, lemon essence, sweet orange essence, lily essence or rose essence) into a mixed solvent of 210-250 mL of 2-methoxyethanol and 120-150 mL of deionized water, and stirring at room temperature for 10-30 min; then adding a mixture of 2.5-3.0 mg of hexadecyl trimethyl ammonium bromide and 2.1-2.5 mg of dodecyl trimethyl ammonium bromide, adjusting the pH value to 11-13 by using 0.1mol/L sodium hydroxide solution, and stirring for 20-40min at room temperature to obtain an alkaline system;
the steps (1) and (2) are not sequenced;
(3) adding the alkaline system obtained in the step (2) into the SiO obtained in the step (1)2Stirring the sol for 24 hours at room temperature, adding the obtained suspension into deionized water, carrying out ultrasonic treatment for 10-20 min, washing and centrifuging for multiple times until the pH value of the supernatant is close to neutral; the centrifugal rotating speed is 3500-6000 r/min, and the time is 10-20 min; obtaining a solid substance;
(4) adding the solid obtained in the step (3) into 75 wt% ethanol water solution, wherein the adding amount of the 75 wt% ethanol is 50-100 of the mass of the solid, stirring for 2-3 h, and performing suction filtration to obtain a solid; repeating the step for 2-3 times, and vacuum drying the solid to obtain heat-resistant essence microcapsule; vacuum drying at 40-50 ℃ for 24-48 h.
And (3) carrying out thermogravimetric analysis on the prepared heat-resistant essence microcapsule, wherein the temperature of the thermogravimetric analysis is 50-120 ℃, and judging the release temperature and the release amount of the essence in the microcapsule.
The heat-resistant essence microcapsule prepared by the preparation method is used in tobacco products, and can ensure stable aroma and lasting and uniform aroma.
The invention has the beneficial effects that:
1. the preparation method of the invention takes mixed surfactant as template agent, 2-methoxy ethanol and water as cosolvent, sodium hydroxide as catalyst, and ethyl orthosilicate as precursor to prepare SiO2Sol, a material prepared by a sol-gel process, has a porous network structure.
2. The heat-resistant essence microcapsule prepared by the preparation method has the characteristics of stable aroma and lasting aroma at the temperature of about 90 ℃. When the perfume is used in tobacco products, the perfume release is stable, the perfume is kept for a long time and is uniform, and the utilization rate of the essence is obviously improved.
3. The preparation method of the invention removes the template agent by extraction method, and retains the essence in the microcapsule. The preparation method of the essence microcapsule is simple, and the prepared essence microcapsule has high essence utilization rate.
Drawings
FIG. 1 is a thermogravimetric analysis curve of essence. Curve A is the thermogravimetric curve of menthol; the curve b is the thermogravimetric curve of the heat-resistant perfume microcapsule prepared in example 1.
Detailed Description
The process of the present invention is further illustrated below with reference to examples, but the scope of the present invention is not limited thereto.
Example 1: preparing the menthol heat-resistant essence microcapsule.
(1) Mixing 50mL of ethyl orthosilicate, 30mL of 0.1mol/L sodium hydroxide and 30mL of absolute ethyl alcohol, stirring at room temperature, dropwise adding 30mL of 50 wt% ethanol aqueous solution for hydrolysis-polycondensation reaction, heating to 70 ℃ after reaction for 1h, and polymerizing for 2h at constant temperature to obtain SiO2Sol;
(2) adding 1g of menthol into a mixed solvent of 210mL of 2-methoxyethanol and 120mL of deionized water, and stirring for 10min at room temperature; adding 2.5mg of hexadecyl trimethyl ammonium bromide and 2.1mg of dodecyl trimethyl ammonium bromide mixed surfactant, adjusting the pH value to 11-13 by using 0.1mol/L sodium hydroxide solution, and stirring for 20min at room temperature to obtain an alkaline system;
the steps (1) and (2) are not sequenced;
(3) SiO prepared in the step (1)2Adding the sol into the alkaline system obtained in the step (2), stirring for 24h at room temperature to obtain a suspension, adding deionized water into the suspension, performing ultrasonic treatment for 10min, centrifuging for 20min at 3500r/min to obtain a solid, washing the solid with deionized water, performing centrifugal separation, washing and centrifuging for multiple times until the pH value of a supernatant is close to neutral, and obtaining the solid;
(4) adding the solid obtained in the step (3) into 75 wt% ethanol aqueous solution with the weight 50 times that of the solid, stirring for 2 hours, then carrying out suction filtration to obtain the solid, and repeating the step for 2-3 times; vacuum drying the obtained solid at 40-50 ℃ for 24-48 h to obtain the heat-resistant essence microcapsule;
(5) and (4) carrying out thermogravimetric analysis on the heat-resistant essence microcapsules obtained in the step (4), wherein the temperature of the thermogravimetric analysis is 50-120 ℃, and the result of the thermogravimetric analysis is shown in figure 1. FIG. 1 is a thermogravimetric analysis curve of essence, wherein a curve is a thermogravimetric curve of menthol; the curve b is the thermogravimetric curve of the heat-resistant perfume microcapsule prepared in example 1. As can be seen from the curve a in FIG. 1, the decomposition of menthol is severe, the essence begins to lose weight severely at about 67 ℃, and when the temperature reaches 110 ℃, the weight loss rate reaches 82%; as can be seen from the b curve of fig. 1, there was a slight loss of the essence of the capsule before 110 ℃, which was caused by the residual solvent in the sample and the attached essence on the surface; the temperature is 110-125 ℃, the heat weight loss of the capsule essence is the highest, the temperature reaches the melting point of the wall material, and the capsule essence starts to be gradually decomposed along with the increase of the temperature. Therefore, as can be seen from fig. 1, the heat-resistant essence microcapsule prepared in this example has less component loss at a temperature lower than 110 ℃; the essence begins to volatilize from 110 ℃, and the essence volatilizes to reach the balance when the temperature reaches 150 ℃. The heat-resistant effect of the prepared heat-resistant essence microcapsule is obviously improved.
The prepared heat-resistant essence microcapsule is used in tobacco products, so that the aroma is stable, and the aroma is lasting and uniform.
Example 2: preparation of lemon essence heat-resistant essence microcapsule
(1) Same as example 1, step (1);
(2) adding 2g of lemon essence into a mixed solvent of 250mL of 2-methoxyethanol and 150mL of deionized water, and stirring for 20min at room temperature; adding 3.0mg of hexadecyl trimethyl ammonium bromide and 2.5mg of dodecyl trimethyl ammonium bromide mixed surfactant, adjusting the pH value to 11-13 by using 0.1mol/L sodium hydroxide solution, and stirring for 30min at room temperature;
the steps (1) and (2) are not sequenced;
(3) SiO prepared in the step (1)2Adding the sol into the step (2), stirring for 24h at room temperature to obtain a suspension, adding deionized water into the suspension, carrying out ultrasonic treatment for 15min, centrifuging for 15min at 5000r/min to obtain a solid, washing the solid with deionized water, then carrying out centrifugal separation, washing and centrifuging for multiple times until the pH value of a supernatant is close to neutral, and obtaining the solid;
(4) adding 50 times of 75 wt% ethanol into the solid obtained in the step (3), stirring for 2h, then performing suction filtration to obtain the solid, and repeating the step for 2-3 times; vacuum drying the obtained solid at 40-50 ℃ for 24-48 h to obtain the heat-resistant essence microcapsule;
(5) and (4) carrying out thermogravimetric analysis on the heat-resistant essence microcapsule obtained in the step (4), wherein the temperature of the thermogravimetric analysis is 50-120 ℃. The result is less loss of components at temperatures below 115 ℃; the essence begins to volatilize from 115 ℃, and the essence volatilizes to reach the balance when the temperature reaches 160 ℃. The heat-resistant effect of the prepared heat-resistant essence microcapsule is obviously improved.
The prepared heat-resistant essence microcapsule is used in tobacco products, so that the aroma is stable, and the aroma is lasting and uniform.
Example 3: preparing the lily essence heat-resistant essence microcapsule.
(1) Same as example 1, step (1);
(2) adding 1.5g of lily essence into a mixed solvent of 230mL of 2-methoxyethanol and 130mL of deionized water, and stirring at room temperature for 30 min; adding 2.8mg of hexadecyl trimethyl ammonium bromide and 2.3mg of dodecyl trimethyl ammonium bromide mixed surfactant, adjusting the pH value to 11-13 by using 0.1mol/L sodium hydroxide solution, and stirring for 40min at room temperature;
(3) SiO prepared in the step (1)2Adding the sol into the step (2), stirring for 24h at room temperature to obtain a suspension, adding deionized water for ultrasonic treatment for 20min, centrifuging at 6000r/min for 10min to obtain a solid, washing the solid with deionized water, then performing centrifugal separation, washing and centrifuging for multiple times until the pH value of a supernatant is close to neutral to obtain the solid;
(4) adding 50 times of 75 wt% ethanol into the solid obtained in the step (3), stirring for 2h, then performing suction filtration to obtain the solid, and repeating the step for 2-3 times; vacuum drying the obtained solid at 40-50 ℃ for 24-48 h to obtain the heat-resistant essence microcapsule;
(5) and (4) carrying out thermogravimetric analysis on the heat-resistant essence microcapsule obtained in the step (4), wherein the temperature of the thermogravimetric analysis is 50-120 ℃. The result is less loss of components at temperatures below 120 ℃; the essence begins to volatilize from 120 ℃, and the essence volatilizes to reach the balance when the temperature reaches 160 ℃. The heat-resistant effect of the prepared heat-resistant essence microcapsule is obviously improved.
The prepared heat-resistant essence microcapsule is used in tobacco products, so that the aroma is stable, and the aroma is lasting and uniform.
Claims (2)
1. A preparation method of heat-resistant essence microcapsules is characterized in that the heat-resistant essence microcapsules begin to volatilize essence from 120 ℃ and reach the balance of essence volatilization at 160 ℃, and comprises the following steps:
(1) mixing 50mL of ethyl orthosilicate, 30mL of 0.1mol/L sodium hydroxide and 30mL of absolute ethyl alcohol, stirring at room temperature, dropwise adding 30mL of 50 wt% ethanol aqueous solution for hydrolysis-polycondensation reaction, heating to 70 ℃ after reaction for 1h, and polymerizing for 2h at constant temperature to obtain SiO2Sol;
(2) adding 1.5g of lily essence into a mixed solvent of 230mL of 2-methoxyethanol and 130mL of deionized water, and stirring at room temperature for 30 min; adding 2.8mg of hexadecyl trimethyl ammonium bromide and 2.3mg of dodecyl trimethyl ammonium bromide mixed surfactant, adjusting the pH value to 11-13 by using 0.1mol/L sodium hydroxide solution, and stirring for 40min at room temperature;
(3) SiO prepared in the step (1)2Adding the sol into the step (2), stirring for 24h at room temperature to obtain a suspension, adding deionized water into the suspension, carrying out ultrasonic treatment for 20min, centrifuging at 6000r/min for 10min to obtain a solid, washing the solid with deionized water, then carrying out centrifugal separation, washing and centrifuging for multiple times until the pH value of a supernatant is close to neutral to obtain the solid;
(4) adding 50 times of 75 wt% ethanol into the solid obtained in the step (3), stirring for 2h, then performing suction filtration to obtain the solid, and repeating the step for 2-3 times; and (3) drying the obtained solid substance at 40-50 ℃ in vacuum for 24-48 h to obtain the heat-resistant essence microcapsule.
2. Use of heat-resistant flavor microcapsules prepared according to the preparation method of claim 1 in tobacco products.
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| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN103328621B (en) * | 2011-07-04 | 2014-07-02 | 丽华（广州）香精有限公司 | Nano-flavor and preparation method thereof |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
| CN104449590A (en) * | 2014-12-05 | 2015-03-25 | 中国工程物理研究院化工材料研究所 | Phase-change energy-storage material nanocapsule and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103328621B (en) * | 2011-07-04 | 2014-07-02 | 丽华（广州）香精有限公司 | Nano-flavor and preparation method thereof |
| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
| CN104449590A (en) * | 2014-12-05 | 2015-03-25 | 中国工程物理研究院化工材料研究所 | Phase-change energy-storage material nanocapsule and preparation method thereof |
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