CN114908574B - Water-based essence microcapsule and preparation method thereof - Google Patents
Water-based essence microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention provides a water-based essence microcapsule and a preparation method thereof, wherein glutaraldehyde is used as a cross-linking agent, gelatin and chitosan are used as capsule walls, water-soluble essence is used as a capsule core substance, and the prepared water-based essence microcapsule has the advantage of prolonging the fragrance retention time, and solves the problems of easy volatilization, poor thermal stability and short fragrance retention time of essence.
Description
Technical Field
The invention relates to the technical field of essence preparation, in particular to an aqueous essence microcapsule and a preparation method thereof.
Background
Based on the improvement of the living standard of people, the pursuit of the fabrics is not limited to quality, but also has more requirements on the versatility of the fabrics. In one aspect, it is desirable to have fragrance on the fabric garment to maintain pleasure in the fabric garment itself. Early days, fabrics or materials containing fragrances were mixed with fabrics by adsorption methods to volatilize the fragrance into the pores of the fibers, or were impregnated directly with a solution containing perfume, or were flavored by adding a fragrance to the binder and using a coating. However, the method is used for perfuming the fabric, the fragrance retention time is short, and the fragrance is quickly lost after the fabric is washed for several times. Based on the problems of quick volatilization of essence, poor thermal stability and short fragrance retention time, how to slowly release fragrance becomes a technical problem in the technical field.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides an aqueous essence microcapsule and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the water-based essence microcapsule comprises a wall material and a capsule core material, and is characterized in that the wall material is a polymer formed by crosslinking xylitol/glutaraldehyde and gelatin/chitosan, the capsule core material is a water-based essence material, and the chemical structural formula of the polymer is shown as formula (I):
in the formula (I), R1 to R9 are selected from eighteen different amino acids of glycine, alanine, serine, aspartic acid, glutamic acid amino, proline, arginine, histidine, tyrosine, cystine, leucine, threonine, methionine, valine, phenylalanine, tryptophan, glutamic acid and lysine.
Preferably, in the formula (I):
r5 and R6 are selected from eighteen residues of different amino acids glycine, alanine, serine, aspartic acid, glutamine amino, proline, arginine, histidine, tyrosine, cystine, leucine, threonine, methionine, valine, phenylalanine, tryptophan, glutamic acid and lysine;
r3 and R7 are residues of lysine or arginine;
r2, R4 and R8 are residues of aspartic acid or glutamic acid amino;
r1 and R9 are serine, threonine or tyrosine residues.
Preferably, the aqueous essence material consists of oil-soluble essence, modified starch, an emulsifier, a co-emulsifier, a thickener, citric acid, potassium sorbate and distilled water.
Preferably, the oil-soluble essence is one or more of lemon oil essence, floral essence and fruit essence, the emulsifying agent is sucrose ester or polyglycerol ester, the auxiliary emulsifying agent is one or more of ethanol, glycerol or polyethylene glycol, and the thickening agent is xanthan gum or acacia.
Preferably, the aqueous essence material consists of dealdehydized ethanol, white lemon oil, linalool, borneol acetate, terpineol, levocarvone, geranyl acetate, longleaf acetate and propylene glycol.
The invention also provides a preparation method of the water-based essence microcapsule, which specifically comprises the following steps:
a. dissolving gelatin in acetic acid to obtain gelatin acetic acid solution;
b. adding chitosan into gelatin acetic acid solution, stirring to dissolve chitosan to obtain gelatin/chitosan mixed solution, and regulating pH to 5.8-6.2;
c. adding water-soluble essence substances into the gelatin/chitosan mixed solution, and uniformly stirring to obtain a gelatin/chitosan mixed solution containing essence;
d. lecithin is added into vegetable oil as an emulsifying agent, and the mixture is stirred uniformly after heating;
e. adding the gelatin/chitosan mixed solution containing the essence prepared in the step c into the vegetable oil after the step d for heating and emulsifying, closing heating after the emulsification is completed, and naturally cooling to room temperature;
f. adding glutaraldehyde solution into the solution system after the step e for crosslinking reaction, and completely reacting at room temperature;
g. adding xylitol and glacial acetic acid into the reaction system after the step f, regulating the pH to 2-3, and adding N into the reaction system 2 And (3) carrying out crosslinking reaction again under the protection, and obtaining the xylitol/glutaraldehyde double-crosslinked aqueous essence microcapsule after full reaction.
Preferably, the step g further includes:
h. and (c) standing the reaction system obtained in the step (g), removing the upper oil phase, centrifuging, and separating the oil phase to obtain the xylitol-glutaraldehyde double-crosslinked aqueous essence microcapsule.
Preferably, in the step b, when chitosan is added into the gelatin acetic acid solution, the mass ratio of gelatin to chitosan is 10:1, and the pH is preferably adjusted to 6.
Preferably, in the step d, the vegetable oil is one or more of corn oil, olive oil, soybean oil and peanut oil; the emulsification temperature is 35-45 ℃, the emulsification time is 30-60min, and the stirring speed is 500-650rpm; the specific steps of the step f are as follows: adding glutaraldehyde water solution with the volume ratio of 5% into the solution system after the step e, and fully reacting for 5 hours at room temperature, wherein the specific steps of the step g are as follows: adding xylitol into the reaction system in the step f, and addingAdding glacial acetic acid, adjusting pH to 2-3, and adding N 2 And (3) under the protection, the reaction temperature is raised to 40 ℃, after the reaction is carried out for 8 hours, the reaction is cooled to room temperature, and the xylitol/glutaraldehyde double-crosslinked aqueous essence microcapsule is obtained.
Preferably, the weight ratio of each component is as follows: 12-32 parts of gelatin, 1.2-3.2 parts of chitosan, 160-300 parts of 1.0% acetic acid solution, 20-80 parts of aqueous essence solution, 15-25 parts of lecithin, 50-150 parts of 5% glutaraldehyde, 45-55 parts of 1% xylitol solution and 800-1200 parts of vegetable oil.
And preferably, 22 parts of gelatin, 2.2 parts of chitosan, 240 parts of 1.0% acetic acid solution, 60 parts of aqueous essence, 20 parts of lecithin, 100 parts of 5% glutaraldehyde, 50 parts of 1.0% xylitol and 1000 parts of vegetable oil.
Still preferably, in the step d, the volume ratio of the water phase to the oil phase is 1:4, the emulsification temperature is 40 ℃, the emulsification time is 60min, and the stirring speed is 600rpm.
Compared with the prior art, the preparation method has the beneficial effects that glutaraldehyde is adopted as a cross-linking agent, gelatin and chitosan are adopted as capsule walls, water-soluble essence is adopted as a capsule core substance, and the prepared water-based essence microcapsule has the advantage of prolonging the fragrance retention time, and solves the problems of easiness in volatilization, poor thermal stability and short fragrance retention time of the essence.
The principle of the invention is as follows: glutaraldehyde and free amino and free hydroxyl on gelatin and chitosan are subjected to crosslinking reaction to form bridging construction of Schiff base structure and hemiacetal structure, so that linear gelatin and chitosan form a three-dimensional network structure, and the stability of the microcapsule is improved. And because of the crosslinking reaction of glutaraldehyde, most of free amino and carboxyl groups on gelatin and chitosan are consumed, and xylitol is adopted for secondary crosslinking of the microcapsules in order to improve the adhesion effect of the microcapsules and fabrics and the stability of the microcapsules. Xylitol is a natural sweetener extracted from plant materials such as birch, oak, corncob, bagasse, etc., and has wide distribution range and is widely used in various fruits, vegetables and grains. The molecule xylitol molecule contains five hydroxyl groups, which are polyhydroxy compounds, and the xylitol and free carboxyl on the wall gelatin undergo esterification reaction to crosslink gelatin molecules, so that the wall strength is improved, and the microcapsule stability is improved. In addition, xylitol molecules are grafted on gelatin molecules, so that the hydroxyl content of the capsule wall is increased, and stronger hydrogen bonding effect can be generated with cellulose in the fabric in the process of finishing the microcapsule and the fabric, so that the adhesion effect of the microcapsule and the fabric is improved, the loss of the microcapsule is reduced, and the aroma and the smell are enhanced.
Drawings
FIG. 1 is an isoelectric point plot of gelatin, chitosan, and chitosan/gelatin of example 1 at different mass ratios;
FIG. 2 is a thermogravimetric plot of gelatin, chitosan, gelatin/chitosan complex, glutaraldehyde-crosslinked gelatin/chitosan, and xylitol/glutaraldehyde double-crosslinked microcapsules.
FIG. 3 is a scanning electron micrograph of the microcapsules prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
EXAMPLE 1 isoelectric point measurement of gelatin, chitosan, gelatin/Chitosan composite
1.1 isoelectric point of gelatin
0.5g of gelatin is weighed, 100ml of deionized water is added, and the mixture is stirred at a water bath temperature of 50 ℃ until the gelatin is completely dissolved, thus obtaining a gelatin solution with the concentration of 0.5%. The pH was adjusted using 0.001mol/L HCl solution and 0.001mol/L NaOH solution, and the conductivity of the gelatin solution at different pH values was recorded using a pH meter and conductivity meter.
1.2 isoelectric point of chitosan
0.5g of chitosan is weighed and added into 100ml of 0.01mol/L HCl solution, and the mixture is stirred at room temperature until the chitosan is completely dissolved, thus obtaining 0.5 percent chitosan solution. The pH of the solution was adjusted using a 0.001mol/L NaOH solution and the conductivity of the gelatin solution at different pH values was recorded using a pH meter and conductivity meter.
1.3 isoelectric point of Chitosan/gelatin composite
100mL of a 1.0% gelatin solution was placed in a beaker and magnetically stirred at a water bath temperature of 50 ℃. Adding a certain volume of 1.0% chitosan solution into the gelatin solution at the temperature of the gelatin solution, and stirring for 1h to obtain a gelatin/chitosan uniform mixed solution. The volume ratio of chitosan to gelatin is respectively as follows: 4:100, 10:100, 20: 100. 50:100, 75:100, 100:100. The pH of the mixed solution was changed using a 1.0% HCl solution and a 0.1mol/L NaOH solution, and the conductivity of the gelatin/chitosan solution was measured at different pH values using a pH meter and a conductivity meter.
The isoelectric points of the gelatin and the chitosan obtained by the measurement according to the method are shown in table 1; isoelectric curves of gelatin, chitosan and chitosan/gelatin with different mass ratios are shown in fig. 1.
TABLE 1 isoelectric points of gelatin, chitosan and Chitosan/gelatin with different mass ratios
Example 2 preparation method of aqueous essence microcapsules
a. Weighing 2.2g of gelatin in a beaker, and dissolving a certain volume of 1.0% acetic acid at the water bath temperature of 37 ℃;
b. adding 0.22g of chitosan into the gelatin solution according to the mass ratio of gelatin to chitosan of 10:1, stirring for dissolving to obtain a uniform gelatin/chitosan mixed solution, and regulating the pH value to 6 by adopting 5.0% ammonia water solution;
in this step, the pH was adjusted to 6 because gelatin is an amphoteric polymer having an isoelectric point of 5.0 and a pH greater than its isoelectric point, and gelatin molecules on gelatin were negatively charged, i.e., -NH 3 + Has a part of and-OH - Conversion to-NH by binding 2 whereby-COO in the gelatin molecule - (negative charge) content is greater than-NH 3 + (positively charged) content, the molecule is negatively charged. When gelatin is in a medium less than the isoelectric point, the gelatin molecule becomes positively charged, i.e. -COO - With a part of-H + Binding to-COOH, whereby-NH in a gelatin molecule 3 + A (positive charge) content of greater than-COO - (negative charge) content, the molecule is positively charged. Therefore, the pH value of the system is regulated to 6, gelatin is negatively charged, chitosan is positively charged due to the protonation of free ammonia genes on the molecules of the chitosan in an acidic medium, and therefore, complex coacervation reaction occurs between the negatively charged gelatin and the positively charged chitosan due to electrostatic interaction; the ionization reaction of gelatin at different pH is shown as the formula:
the protonation reaction process of chitosan in an acidic medium is shown as a formula III:
the complex coacervation reaction of gelatin and chitosan is shown in formula IV:
c. adding 6.0g of water-soluble essence into the gelatin/chitosan mixed solution, and uniformly stirring to obtain a gelatin/chitosan mixed solution containing the essence;
d. taking 100mL of corn oil in a three-neck flask, adding 2.0g of lecithin serving as an emulsifier, heating to 40 ℃, and uniformly stirring, wherein the lecithin is an ionic surfactant containing amphiphilic groups, and is nontoxic and harmless;
e. adding gelatin/chitosan mixed solution into corn oil for emulsification at 600rpm at 40 ℃ for 60min, closing heating, and naturally cooling to room temperature; gelatin can undergo sol-gel transition, swelling dissolution of gelatin occurs at temperatures above 35 ℃, sol-gel occurs at temperatures below 35 ℃. Thereby reducing the temperature to room temperature, being beneficial to forming a relatively fixed shell film of the particles due to gelatin gel, improving the stability of the particles and being beneficial to the next cross-linking reaction;
f. after cooling downAnd (c) adding 10mL of 5% glutaraldehyde solution into the reaction system of the step (e), reacting for 5 hours at room temperature, wherein two aldehyde groups on glutaraldehyde can cause covalent bond crosslinking between molecules and in molecules of linear gelatin or chitosan, so as to form a three-dimensional space network structure. The free amino groups on the gelatin or chitosan molecule react with glutaraldehyde to form an imine bond (Schiff base) cross-linked structure, and simultaneously, the hydroxy groups on hydroxyproline and hydroxylysine on gelatin and the-CH at the C-6 position on chitosan 2 OH can react with glutaraldehyde to form a crosslink of the hemiacetal structure; the reaction process of the glutaraldehyde crosslinked gelatin/chitosan is as follows:
g. and f, adding 5mL of 1.0% xylitol into the reaction system after the step f, adding glacial acetic acid, regulating the pH to 2-3, and reacting for 8 hours at the temperature of 40 ℃ under the protection of N2, and cooling to room temperature to obtain the xylitol secondary crosslinked essence microcapsule. In the process, the free carboxyl on the gelatin and xylitol generate esterification reaction, so that the gelatin can be subjected to secondary crosslinking, the stability of the microcapsule is improved, and meanwhile, the carboxyl on the gelatin is blocked, and the hydroxyl content of the capsule wall is increased; the structural formula of the xylitol/glutaraldehyde double-crosslinked gelatin/chitosan polymer obtained by the reaction is shown as the formula (I):
h. standing the microcapsule obtained by the reaction for 2 hours, depositing gelatin/chitosan microcapsule on the lower layer, pouring corn oil on the upper layer, pouring out the upper oil phase, taking the lower microcapsule, centrifuging, and separating out the oil phase to obtain the water-based essence microcapsule. And finally transferring the microcapsule into a wide-mouth bottle, and sealing and preserving.
As specific embodiments, the aqueous essence materials in this example can be prepared by the following two formulations:
10.00-60.00 parts of oil-soluble essence (one or more of lemon oil essence, flower-fragrance essence and fruit-fragrance essence); 0.10-2.00 parts of modified starch; 15.00-50.00 parts of sucrose ester and polyglycerol ester (sucrose ester: polyglycerol ester=1:1-1:10) are adopted as the emulsifier; 5.00-25.00 parts of auxiliary emulsifier (ethanol/glycerol/polyethylene glycol, any one of which is adopted); 0.05-0.40 parts of thickening agent (xanthan gum/acacia, any one of which is adopted); 0.01-0.10 parts of citric acid; 0.02-0.08 part of potassium sorbate; distilled water 1.00-5.00 parts.
25.0-30.0 parts of dealdehydized ethanol; 20.0-25.0 parts of essential oil (one or more of fruit-flavor essential oil and flower-flavor essential oil); 2.0-3.0 parts of linalool; 0.1-1.0 part of borneol acetate; 3.0-4.0 parts of terpineol; 4.0-5.0 parts of levo-carvone; 3.0-4.0 parts of geranyl acetate; 1.0 to 2.0 parts of longleaf acetate; 35.0-40.0 parts of propylene glycol.
EXAMPLE 3 gelatin/Chitosan ratio
Table 2 shows the tensile strength and elongation at break of gelatin/chitosan composite films of different mass ratios. As can be seen in table 2, the tensile strength of the pure-bright adhesive film was 288.69MPa and the elongation at break was 6.05%; the tensile strength of the pure chitosan film is 201.62MPa, and the elongation at break is 11.61%. When the two are mixed in proportion, the tensile strength of the composite film is higher than that of the pure chitosan film, but the elongation at break is lower than that of the pure gelatin film or the pure chitosan film. In the composite film, the highest tensile strength was 282.53MPa when the ratio of gelatin to chitosan was 10:1, but at the same time the lowest elongation at break was 2.03%. As the proportion of chitosan increases, the tensile strength of the composite film decreases while the elongation at break increases.
TABLE 2 mechanical Properties of composite films with different gelatin/Chitosan ratios
Example 4 thermogravimetric analysis (TG)
3.1 analytical method
2-6mg of sample is weighed, and is tested by adopting a TG/DSC synchronous thermal analyzer, the temperature is raised from room temperature to 600 ℃ at the speed of 10 ℃/min, and the gas atmosphere is nitrogen.
3.2 analysis results
The thermal decomposition temperatures of the different samples are shown in table 2,
TABLE 2 thermal decomposition temperatures of different samples
Fig. 2 is a graph of thermal weight curves of gelatin, chitosan, gelatin/chitosan complex, glutaraldehyde crosslinked gelatin/chitosan and xylitol/glutaraldehyde double crosslinked gelatin/chitosan, and as can be seen from table 2 and fig. 2, the thermal decomposition temperature of xylitol/glutaraldehyde double crosslinked gelatin/chitosan is maximum, reaching 329 ℃, and the thermal stability is higher than that of glutaraldehyde primary crosslinked gelatin/chitosan. Therefore, the microcapsule crosslinked film subjected to xylitol secondary crosslinking has better thermal stability.
The reason for the above results is that: in this patent example 2, the double cross-linking agent is adopted, glutaraldehyde is adopted for the first cross-linking, xylitol is adopted for the second cross-linking, and gelatin/chitosan on the microcapsule wall can be further cross-linked and solidified, so that the strength of the microcapsule wall is improved, and the thermal stability of the microcapsule is increased.
Example 5 field emission Scanning Electron Microscope (SEM)
Fixing a small amount of powder sample with conductive adhesive, performing metal spraying treatment, and observing the particle size and morphology of the microcapsule by adopting a JSM-7800F field emission scanning electron microscope.
FIG. 3 is a scanning electron micrograph of the prepared xylitol/glutaraldehyde double-crosslinked aqueous essence microcapsule, wherein the xylitol and glutaraldehyde double-crosslinked gelatin/chitosan microcapsule has a spherical shape, a rough surface, a particle size of about 40 μm and a uniform particle size distribution.
EXAMPLE 6 analysis of results
According to the invention, glutaraldehyde is used as a cross-linking agent, gelatin and chitosan are used as capsule walls, water-soluble essence is used as a capsule core, the gelatin/chitosan essence microcapsule is prepared, the essence is microencapsulated, the fragrance retention time is prolonged, and the problems of easiness in volatilization, poor thermal stability and short fragrance retention time of the essence are solved. Glutaraldehyde and free amino and free hydroxyl of gelatin and chitosan are subjected to crosslinking reaction to form bridging construction of Schiff base structure and hemiacetal structure, so that linear gelatin and chitosan form a three-dimensional network structure, and the stability of the microcapsule is improved. And because of the crosslinking reaction of glutaraldehyde, most of free amino and carboxyl of gelatin and chitosan are consumed, and xylitol is adopted for secondary crosslinking of the microcapsules in order to improve the adhesion of the microcapsules to fabrics and the stability of the microcapsules. Xylitol is a natural sweetener extracted from plant materials such as birch, oak, corncob, bagasse, etc., and widely exists in various fruits, vegetables, and grains. The molecule xylitol molecule contains five hydroxyl groups, which are polyhydroxy compounds, and the xylitol and free carboxyl on the wall gelatin undergo esterification reaction to crosslink gelatin molecules, so that the wall strength is improved, and the microcapsule stability is improved. In addition, xylitol molecules are grafted on gelatin molecules, so that the hydroxyl content of the capsule wall is increased, and stronger hydrogen bonding effect can be generated with cellulose in the fabric in the process of finishing the microcapsule and the fabric, so that the adhesion effect of the microcapsule and the fabric is improved, the loss of the microcapsule is reduced, and the aroma and the smell are enhanced.
In the invention, the principle of hydrogen bond interaction between cellulose and hydroxyl groups on the crosslinked capsule wall is shown as follows:
the foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should be covered by the protection scope of the present invention by equally replacing or changing the technical scheme and the inventive concept thereof.
Claims (10)
1. The water-based essence microcapsule comprises a wall material and a capsule core material, and is characterized in that the wall material is a polymer formed by crosslinking xylitol/glutaraldehyde and gelatin/chitosan, the capsule core material is a water-based essence material, and the chemical structural formula of the polymer is shown as formula (I):
in the formula (I), R is 1 To R 9 One of the residues selected from eighteen different amino acids glycine, alanine, serine, aspartic acid, glutamic acid amino, proline, arginine, histidine, tyrosine, cystine, leucine, threonine, methionine, valine, phenylalanine, tryptophan, glutamic acid and lysine.
2. The aqueous perfume micro-capsule of claim 1, wherein: in the formula (I):
R 5 、R 6 residues selected from eighteen different amino acids glycine, alanine, serine, aspartic acid, glutamic acid amino group, proline, arginine, histidine, tyrosine, cystine, leucine, threonine, methionine, valine, phenylalanine, tryptophan, glutamic acid and lysine;
R 3 、R 7 residues that are lysine or arginine;
R 2 、R 4 、R 8 residues that are aspartic acid or glutamic acid amino groups;
R 1 、R 9 residues that are serine, threonine or tyrosine.
3. The aqueous perfume micro-capsule of claim 1, wherein: the water-based essence substance consists of oil-soluble essence, modified starch, an emulsifier, a co-emulsifier, a thickener, citric acid, potassium sorbate and distilled water.
4. A water-based essence microcapsule according to claim 3, characterized in that: the oil-soluble essence is one or more of lemon oil essence, floral essence and fruit essence, the emulsifying agent is sucrose ester or polyglycerol ester, the auxiliary emulsifying agent is one or more of ethanol, glycerol or polyethylene glycol, and the thickening agent is xanthan gum or acacia.
5. The aqueous perfume micro-capsule of claim 1, wherein: the water-based essence substance consists of dealdehydized ethanol, white lemon oil, linalool, borneol acetate, terpineol, levo-carvone, geranyl acetate, longleaf acetate and propylene glycol.
6. The preparation method of the water-based essence microcapsule specifically comprises the following steps:
a. dissolving gelatin in acetic acid to obtain gelatin acetic acid solution;
b. adding chitosan into gelatin acetic acid solution, stirring to dissolve chitosan to obtain gelatin/chitosan mixed solution, and regulating pH to 5.8-6.2;
c. adding water-soluble essence substances into the gelatin/chitosan mixed solution, and uniformly stirring to obtain a gelatin/chitosan mixed solution containing essence;
d. lecithin is added into vegetable oil as an emulsifying agent, and the mixture is stirred uniformly after heating;
e. adding the gelatin/chitosan mixed solution containing the essence prepared in the step c into the vegetable oil after the step d for heating and emulsifying, closing heating after the emulsification is completed, and naturally cooling to room temperature;
f. adding glutaraldehyde solution into the solution system after the step e for crosslinking reaction, and completely reacting at room temperature;
g. adding xylitol and glacial acetic acid into the reaction system after the step f, regulating the pH to 2-3, and adding N into the reaction system 2 And (3) carrying out crosslinking reaction again under the protection, and obtaining the xylitol/glutaraldehyde double-crosslinked aqueous essence microcapsule after full reaction.
7. The method for preparing the aqueous essence microcapsule according to claim 6, wherein the step g further comprises:
h. and (c) standing the reaction system obtained in the step (g), removing the upper oil phase, centrifuging, and separating the oil phase to obtain the xylitol-glutaraldehyde double-crosslinked aqueous essence microcapsule.
8. The method for preparing the aqueous essence microcapsule according to claim 6, wherein in the step b, when chitosan is added into the gelatin acetic acid solution, the mass ratio of gelatin to chitosan is 10:1, and preferably the pH is adjusted to 6.
9. The method for preparing the aqueous essence microcapsule according to claim 6, wherein in the step d, the vegetable oil is one or more of corn oil, olive oil, soybean oil and peanut oil; the emulsification temperature is 35-45 ℃, the emulsification time is 30-60min, and the stirring speed is 500-650rpm; the specific steps of the step f are as follows: adding glutaraldehyde water solution with the volume ratio of 5% into the solution system after the step e, and fully reacting for 5 hours at room temperature, wherein the specific steps of the step g are as follows: adding xylitol and glacial acetic acid into the reaction system of the step f, regulating the pH to 2-3, and adding N 2 And (3) under protection, the reaction temperature is increased to 40 ℃, after the reaction is carried out for 8 hours, the reaction is cooled to room temperature, and the xylitol/glutaraldehyde double-crosslinked aqueous essence microcapsule is obtained.
10. The preparation method of the aqueous essence microcapsule according to claim 6, wherein the components are mixed according to mass fraction: 12-32 parts of gelatin, 1.2-3.2 parts of chitosan, 160-300 parts of 1.0% acetic acid solution, 20-80 parts of aqueous essence solution, 15-25 parts of lecithin, 50-150 parts of 5% glutaraldehyde, 45-55 parts of 1% xylitol solution and 800-1200 parts of vegetable oil.
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| CN112827436A (en) * | 2020-12-22 | 2021-05-25 | 天津科技大学 | Preparation method of chitosan/cellulose nanocrystal slow-release essence microcapsule |
| CN113088395A (en) * | 2021-05-10 | 2021-07-09 | 云南中烟工业有限责任公司 | Wild plum microcapsule for cigarettes and preparation method thereof |
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| US3956172A (en) * | 1972-07-19 | 1976-05-11 | Fuji Photo Film Co., Ltd. | Process for hardening microcapsules containing hydrophobic oil droplets |
| CN102039108A (en) * | 2011-01-13 | 2011-05-04 | 广州市戴文高分子材料科技有限公司 | Preparation method of essence microcapsules |
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| CN113088395A (en) * | 2021-05-10 | 2021-07-09 | 云南中烟工业有限责任公司 | Wild plum microcapsule for cigarettes and preparation method thereof |
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