CN111972423B - Bactericidal agent suitable for menthol and preparation method thereof - Google Patents
Bactericidal agent suitable for menthol and preparation method thereof Download PDFInfo
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- CN111972423B CN111972423B CN202010771967.5A CN202010771967A CN111972423B CN 111972423 B CN111972423 B CN 111972423B CN 202010771967 A CN202010771967 A CN 202010771967A CN 111972423 B CN111972423 B CN 111972423B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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Abstract
The invention relates to a menthol production process, and provides a sterilizing agent suitable for menthol aiming at the problem of poor natamycin solubility and stability, wherein the main component is natamycin, the surface of the natamycin is coated with hydroxypropyl-beta-cyclodextrin, and the coated natamycin is loaded on MCM-41. The hydroxypropyl-beta-cyclodextrin can improve the water solubility and enhance the stability of natamycin; MCM-41 adsorbs the coated natamycin, enriches the natamycin, increases the concentration of the natamycin, can improve the sterilization effect, is beneficial to the separation and recovery of sterilizing agents, improves the specific surface area of the loaded natamycin, enables yeast or fungi to gather on the surface of the natamycin, and can further improve the sterilization effect. The invention also provides a preparation method of the sterilizing agent suitable for menthol.
Description
Technical Field
The invention relates to a production process of menthol, in particular to a sterilizing agent suitable for the menthol and a preparation method thereof.
Background
The total number of the mould and the microzyme in the menthol is not more than 100cfu/g, and the menthol is required to be sterilized to meet the safety requirement. Natamycin is a strong broad-spectrum antifungal agent, and can effectively inhibit the growth of fungi such as yeast. At present, natamycin is approved as a natural biological preservative for the production and preservation of certain dairy products, meats, beverages, fruits and many other food products. For example, chinese patent publication No. CN111387253A discloses a natural cake fresh-keeping additive, which can significantly prolong the fresh-keeping time of cake by adding 0.1-0.3 parts of natamycin.
Due to the existence of two typical configurations on natamycin structure: the enol-structure and the keto-structure, which determine the disadvantage of low solubility in many solvents. The solubility of natamycin in water at room temperature is 30-50 mg/L. At present, the natamycin serving as a food preservative is mainly used for treating the surface of food, because the dissolved natamycin can only be combined with a target substance to play a role, the low water solubility of the natamycin is not beneficial to the utilization of the natamycin, the using effect of the natamycin is seriously influenced, and the using range of the natamycin is also limited. And natamycin is greatly influenced by temperature, ultraviolet light, oxidant and the like. It is hereby necessary to treat natamycin to make it suitable for menthol sterilisation.
Disclosure of Invention
The invention provides a sterilizing agent suitable for menthol and a preparation method thereof in order to overcome the problem of poor solubility and stability of natamycin.
In order to achieve the purpose, the invention adopts the following technical scheme:
a sterilizing agent suitable for menthol comprises natamycin as main ingredient, wherein the surface of the natamycin is coated with hydroxypropyl-beta-cyclodextrin, and the coated natamycin is loaded on MCM-41.
The main component of the sterilizing agent is natamycin, and the natamycin can effectively eliminate yeast and mould in the menthol. However, natamycin can only be combined with a target substance to play a role, and the low water solubility of natamycin is not beneficial to the natamycin to play a sterilization effect, so that the surface of the natamycin is coated with hydroxypropyl-beta-cyclodextrin, and the hydroxypropyl-beta-cyclodextrin has the characteristics of internal hydrophobicity and external hydrophilicity so that the natamycin can be coated on the surface of the natamycin, thereby improving the water solubility and reducing the influence of the natamycin on temperature, ultraviolet light, oxidant and the like. MCM-41 has narrow pore distribution and large specific surface area, can adsorb the coated natamycin, enrich the natamycin and increase the concentration of the natamycin, thus not only improving the sterilization effect, but also being beneficial to the separation and recovery of sterilizing agents. On the other hand, compared with independently dispersed natamycin particles, the specific surface area of the loaded natamycin is improved, so that yeast or fungi are gathered on the surface of the natamycin, and the sterilization effect can be further improved. MCM-41 is an array formed by hexagonal close packing of one-dimensional linear pore channels, and compared with a three-dimensional pore channel structure, the contact of natamycin and the outside is not influenced to play a sterilization role.
The invention also provides a preparation method of the sterilizing agent for menthol, which comprises the following steps:
(1) dissolving natamycin in an alkaline solution with the pH value of 12-13, adding hydroxypropyl-beta-cyclodextrin with the amount of 2-4 times of that of a natamycin substance, carrying out inclusion reaction with the natamycin at 20-40 ℃, neutralizing and drying after the reaction is finished, thus obtaining natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) dispersing natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and MCM-41 molecular sieve in water, stirring for 3-5h, filtering, washing and drying to obtain the sterilizing agent.
Preferably, the preparation method of the MCM-41 molecular sieve comprises the following steps: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 8-9 with acid, stirring to make the solution become gel, adding CTAB, and making the molar ratio of each substance be SiO2:CTAB:H2Stirring for 1-2h, placing the mixture into a reaction kettle, crystallizing at the temperature of 130-150 ℃ for 2-4d, cooling to room temperature, performing suction filtration, washing and drying to obtain molecular sieve raw powder, and roasting to obtain the MCM-41 molecular sieve.
Preferably, the roasting process is as follows: firstly standing at room temperature for 30min, then heating to 100 ℃, keeping the temperature for 1h, then heating to 500-550 ℃ at the speed of 5-8 ℃/min, and keeping the temperature for 4-6 h.
Preferably, the surface of the MCM-41 molecular sieve is modified by carboxyl, and the preparation method comprises the following steps:
dissolving propyl triethoxysilane in tetrahydrofuran, adding the MCM-41 molecular sieve, reacting at 20-25 ℃ for 5-8h, centrifugally washing, and drying to obtain the amino modified MCM-41 molecular sieve;
adding the amino modified MCM-41 molecular sieve into a DMSO solution of succinic anhydride and triethylamine, wherein the mass ratio of the amino modified MCM-41 molecular sieve to the succinic anhydride to the triethylamine is 100 (40-60) to (40-60), stirring for 1-2 days at 40-60 ℃, centrifuging, and washing with ethanol to obtain the carboxyl modified MCM-41 molecular sieve.
The MCM-41 molecular sieve and the natamycin-hydroxypropyl-beta-cyclodextrin inclusion compound are physically adsorbed, so that the attraction is limited, the falling possibility exists, and the stability of the sterilizing agent is influenced. Considering that the natamycin-hydroxypropyl-beta-cyclodextrin inclusion compound has hydroxyl outside, carboxyl is introduced on the surface of the MCM-41 molecular sieve, and the natamycin-hydroxypropyl-beta-cyclodextrin inclusion compound and the MCM-41 molecular sieve are connected through chemical bonds. And even if the natamycin is exposed after the hydroxypropyl-beta-cyclodextrin is dissolved in water, the hydroxyl of the natamycin can be connected with the carboxyl on the surface of the MCM-41 molecular sieve, so that the separation and the recovery of the sterilizing agent are facilitated. Preferably, the natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and the MCM-41 molecular sieve modified by carboxyl are mixed in an excessive amount, so that the carboxyl reaction of the MCM-41 molecular sieve is completely guaranteed, the reaction of the MCM-41 molecular sieve and the peppermint oil is prevented, and the yield of the peppermint oil is guaranteed.
Preferably, the mass ratio of the amino-modified MCM-41 molecular sieve, the succinic anhydride and the triethylamine in the step (II) is 100:50: 50.
Preferably, the drying condition in the step (2) is vacuum drying at 50-70 ℃.
Therefore, the invention has the following beneficial effects: (1) the surface of the natamycin is coated with the hydroxypropyl-beta-cyclodextrin, and the hydroxypropyl-beta-cyclodextrin has the characteristics of hydrophobic interior and hydrophilic exterior so that the natamycin can be coated on the surface of the natamycin, thereby not only improving the water solubility, but also reducing the influence of temperature, ultraviolet light, oxidant and the like on the natamycin; (2) MCM-41 has narrow pore distribution and large specific surface area, can adsorb the coated natamycin, enrich the natamycin and increase the concentration of the natamycin, thus not only improving the sterilization effect, but also being beneficial to the separation and recovery of sterilizing agents; (3) compared with independently dispersed natamycin particles, the specific surface area of the loaded natamycin is improved, so that yeast or fungi are gathered on the surface of the natamycin, and the sterilization effect can be further improved.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipments used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
A method for preparing a sterilizing agent suitable for menthol comprises the following steps:
(1) dissolving natamycin in a sodium hydroxide solution with the pH value of 12, adding hydroxypropyl-beta-cyclodextrin with the amount of 2 times of that of natamycin, carrying out an inclusion reaction with the natamycin at 40 ℃ by ultrasonic treatment for 5 hours, adding 1mol/L hydrochloric acid for neutralization after the reaction is finished, and drying to obtain natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) preparing an MCM-41 molecular sieve: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 9 with 5mol/L sulfuric acid solution, stirring for 10min to make the solution become gel, adding CTAB, and making the molar ratio of each substance be SiO2:CTAB:H2Stirring for 2h, then placing the mixture into a reaction kettle, crystallizing for 2d at 150 ℃, cooling to room temperature, carrying out suction filtration, washing with distilled water, roasting in air at 260 ℃ for 2h, and roasting at 540 ℃ for 6h to obtain the MCM-41 molecular sieve;
(3) dispersing the natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and the MCM-41 molecular sieve in water, stirring for 3 hours, filtering, washing and drying to obtain the sterilizing agent. The main component of the sterilizing agent is natamycin, the surface of the natamycin is coated with hydroxypropyl-beta-cyclodextrin, and the coated natamycin is loaded on MCM-41.
Example 2
A method for preparing a sterilizing agent suitable for menthol comprises the following steps:
(1) dissolving natamycin in a sodium hydroxide solution with the pH value of 12, adding hydroxypropyl-beta-cyclodextrin with the amount of 2 times of that of natamycin, carrying out an inclusion reaction with the natamycin at 40 ℃ by ultrasonic treatment for 5 hours, adding 1mol/L hydrochloric acid for neutralization after the reaction is finished, and drying to obtain natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) preparing an MCM-41 molecular sieve: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 9 with 5mol/L sulfuric acid solution, stirring to make the solution become gel, adding CTAB, and making the molar ratio of each substance be SiO2:CTAB:H2Stirring for 1h, then placing the mixture into a reaction kettle, crystallizing for 2d at the temperature of 150 ℃, cooling to room temperature, carrying out suction filtration and washing, carrying out vacuum drying at the temperature of 50 ℃ to obtain molecular sieve raw powder, placing the molecular sieve raw powder into a muffle furnace for roasting, specifically, placing the molecular sieve raw powder for 30min at the room temperature, then heating to 100 ℃, keeping the temperature for 1h, then heating to 500 ℃ at the speed of 5 ℃/min, and keeping the temperature for 6h to obtain the MCM-41 molecular sieve;
(3) surface carboxyl modification of the MCM-41 molecular sieve:
dissolving aminopropyltriethoxysilane in tetrahydrofuran, adding the MCM-41 molecular sieve, reacting for 8 hours at 20 ℃, centrifugally washing, and drying to obtain an amino-modified MCM-41 molecular sieve;
adding the amino modified MCM-41 molecular sieve into DMSO solution of succinic anhydride and triethylamine, wherein the mass ratio of the amino modified MCM-41 molecular sieve to the succinic anhydride to the triethylamine is 100:40:40, stirring for 1d at 50 ℃, centrifuging, and washing with ethanol to obtain the carboxyl modified MCM-41 molecular sieve.
(4) And (3) dispersing excessive natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and MCM-41 molecular sieve in water, stirring for 3 hours, filtering, washing and drying to obtain the sterilizing agent.
Example 3
A method for preparing a sterilizing agent suitable for menthol comprises the following steps:
(1) dissolving natamycin in a sodium hydroxide solution with the pH value of 13, adding hydroxypropyl-beta-cyclodextrin with the amount of 3 times of that of the natamycin substance, carrying out an inclusion reaction with the natamycin at 30 ℃ by ultrasonic treatment for 5 hours, adding 1mol/L hydrochloric acid for neutralization after the reaction is finished, and drying to obtain natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) preparing an MCM-41 molecular sieve: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 8 with 5mol/L sulfuric acid solution, stirring to make the solution become gel, adding CTAB, and making the molar ratio of each substance be SiO2:CTAB:H2Stirring for 2h, putting the mixture into a reaction kettle, crystallizing for 3d at 140 ℃, cooling to room temperature, filtering, washing, drying in vacuum at 55 ℃ to obtain molecular sieve raw powder, putting the molecular sieve raw powder into a muffle furnace for roasting, and specifically, putting the molecular sieve raw powder into the muffle furnace at room temperature and putting the molecular sieve raw powder downStanding for 30min, heating to 100 deg.C, maintaining the temperature for 1h, heating to 550 deg.C at a rate of 7 deg.C/min, and maintaining the temperature for 4h to obtain MCM-41 molecular sieve;
(3) surface carboxyl modification of the MCM-41 molecular sieve:
dissolving aminopropyltriethoxysilane in tetrahydrofuran, adding the MCM-41 molecular sieve, reacting for 5 hours at 25 ℃, centrifugally washing, and drying to obtain an amino-modified MCM-41 molecular sieve;
adding the amino modified MCM-41 molecular sieve into DMSO solution of succinic anhydride and triethylamine, wherein the mass ratio of the amino modified MCM-41 molecular sieve to the succinic anhydride to the triethylamine is 100:50:50, stirring for 2d at 40 ℃, centrifuging, and washing with ethanol to obtain the carboxyl modified MCM-41 molecular sieve.
(4) And (3) dispersing excessive natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and MCM-41 molecular sieve in water, stirring for 4 hours, filtering, washing and drying to obtain the sterilizing agent.
Example 4
A preparation method of a sterilizing agent suitable for menthol comprises the following steps:
(1) dissolving natamycin in a sodium hydroxide solution with the pH value of 12, adding hydroxypropyl-beta-cyclodextrin with the amount of 4 times of that of the natamycin substance, carrying out an inclusion reaction with the natamycin at 20 ℃ by ultrasonic treatment for 5 hours, adding 1mol/L hydrochloric acid for neutralization after the reaction is finished, and drying to obtain natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) preparing an MCM-41 molecular sieve: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 8 with 5mol/L sulfuric acid solution, stirring to obtain gel, adding CTAB (cetyltrimethyl ammonium bromide) with molar ratio of SiO2:CTAB:H2Stirring for 1h, then placing the mixture into a reaction kettle, crystallizing for 4d at 130 ℃, cooling to room temperature, carrying out suction filtration and washing, carrying out vacuum drying at 50 ℃ to obtain molecular sieve raw powder, placing the molecular sieve raw powder into a muffle furnace for roasting, specifically, placing the molecular sieve raw powder for 30min at room temperature, then heating to 100 ℃, keeping the temperature for 1h, then heating to 550 ℃ at the speed of 8 ℃/min, and keeping the temperature for 5h to obtain the MCM-41 molecular sieve;
(3) surface carboxyl modification of the MCM-41 molecular sieve:
dissolving aminopropyltriethoxysilane in tetrahydrofuran, adding the MCM-41 molecular sieve, reacting for 7 hours at 22 ℃, centrifugally washing, and drying to obtain an amino-modified MCM-41 molecular sieve;
adding the amino modified MCM-41 molecular sieve into a DMSO solution of succinic anhydride and triethylamine, wherein the mass ratio of the amino modified MCM-41 molecular sieve to the succinic anhydride to the triethylamine is 100:60:60, stirring for 1d at 60 ℃, centrifuging, and washing with ethanol to obtain the carboxyl modified MCM-41 molecular sieve.
(4) And (3) dispersing excessive natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and MCM-41 molecular sieve in water, stirring for 5 hours, filtering, washing and drying to obtain the sterilizing agent.
Comparative example 1
Dissolving natamycin in a sodium hydroxide solution with the pH value of 12, adding hydroxypropyl-beta-cyclodextrin with the amount of 2-time of the natamycin substance, carrying out inclusion reaction with the natamycin at 40 ℃, adding 1mol/L hydrochloric acid for neutralization after the reaction is finished, and drying to obtain natamycin-hydroxypropyl-beta-cyclodextrin inclusion compound powder serving as a sterilizing agent.
Comparative example 2
Dispersing natamycin and the MCM-41 molecular sieve prepared in the step (2) in water, carrying out ultrasonic treatment for 3-5h, filtering, washing and drying to obtain a sterilizing agent.
The use of sterilizing agents: the preparation process of menthol includes primary freeze separation of raw menthol oil to obtain primary menthol and secondary oil, secondary freeze separation of the secondary oil to obtain secondary menthol and hair oil, heating to melt the primary menthol and the secondary menthol with saline water, dewatering, filtering, mixing with dried menthol oil and molten oil, crystallization, drying, airing and packing. In the step of heating and melting the saline water, the sterilizing agent prepared by the invention is added, stirred for 3 hours and then filtered to remove the sterilizing agent.
Performance testing
The total content of mold and yeast in the peppermint oil treated according to the above sterilizing agent method was measured, and the results are shown in the following table.
According to the stipulation, the total number of the mould and the microzyme in the menthol is not more than 100cfu/g, and the sterilizing agent prepared by the invention meets the requirement. As shown in the analysis table, in example 1, compared with examples 2-4, the surface treatment of the MCM-41 molecular sieve is not carried out, and the sterilization effect is slightly inferior, because the surface of the MCM-41 molecular sieve is grafted with carboxyl groups, the connection with the coated natamycin can be enhanced, and the natamycin is not easy to lose. The difference between comparative example 1 and example 1 is that the natamycin is not loaded on the MCM-41 molecular sieve, resulting in poor sterilization effect, which indicates that the specific surface area of the loaded natamycin is increased compared to independently dispersed natamycin particles, and the sterilization effect can be further increased by allowing yeast or fungi to aggregate on the surface thereof. The difference between comparative example 2 and example 1 is that the natamycin has poor solubility and the sterilization effect is naturally poor without coating hydroxypropyl-beta-cyclodextrin.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A sterilizing agent suitable for menthol is characterized in that the main component is natamycin, the surface of the natamycin is coated with hydroxypropyl-beta-cyclodextrin, the coated natamycin is loaded on MCM-41, and the surface of the MCM-41 molecular sieve is modified by carboxyl; the carboxyl modification method comprises the following steps:
dissolving aminopropyltriethoxysilane in tetrahydrofuran, adding the MCM-41 molecular sieve, reacting at 20-25 ℃ for 5-8h, centrifugally washing, and drying to obtain an amino-modified MCM-41 molecular sieve;
adding the amino modified MCM-41 molecular sieve into DMSO solution of succinic anhydride and triethylamine, wherein the mass ratio of the amino modified MCM-41 molecular sieve to the succinic anhydride to the triethylamine is 100 (40-60) to (40-60), stirring for 1-2 days at 40-60 ℃, centrifuging, and washing with ethanol to obtain the carboxyl modified MCM-41 molecular sieve.
2. A method of preparing a sterilizing agent suitable for menthol according to claim 1, comprising the steps of:
(1) dissolving natamycin in an alkaline solution with the pH value of 12-13, adding hydroxypropyl-beta-cyclodextrin with the amount of 2-4 times of that of the natamycin substance, carrying out inclusion reaction with the natamycin at 20-40 ℃, neutralizing and drying after the reaction is finished, thus obtaining natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder;
(2) dispersing the natamycin-hydroxypropyl-beta-cyclodextrin inclusion powder and the MCM-41 molecular sieve in water, stirring for 3-5h, filtering, washing and drying to obtain the sterilizing agent.
3. A method for preparing a sterilizing agent suitable for menthol according to claim 2, wherein the MCM-41 molecular sieve is prepared by: adding sodium silicate into distilled water, heating to dissolve, adjusting pH to 8-9 with acid, stirring to make the solution become gel, adding CTAB, and making the molar ratio of each substance be SiO2:CTAB:H2Stirring for 1-2h, placing the mixture into a reaction kettle, crystallizing at the temperature of 130-150 ℃ for 2-4d, cooling to room temperature, performing suction filtration, washing and drying to obtain molecular sieve raw powder, and roasting to obtain the MCM-41 molecular sieve.
4. The method for preparing a sterilizing agent suitable for menthol according to claim 3, wherein the roasting process comprises: standing at room temperature for 30min, heating to 100 deg.C, holding for 1h, heating to 500-.
5. A preparation method of a sterilizing agent suitable for menthol according to claim 2, wherein the mass ratio of the amino-modified MCM-41 molecular sieve, succinic anhydride and triethylamine in the step (2) is 100:50: 50.
6. A preparation method of sterilizing agent suitable for menthol according to claim 2, wherein the drying condition in step (2) is vacuum drying at 50-70 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102742581A (en) * | 2012-07-20 | 2012-10-24 | 陕西省微生物研究所 | Preparation method of natamycin-hydroxypropyl-beta-cyclodextrin inclusion complex |
| CN105664172A (en) * | 2016-01-19 | 2016-06-15 | 宁夏金太阳药业有限公司 | Preparation method of menthol inclusion compound |
| CN110982620A (en) * | 2019-11-26 | 2020-04-10 | 云南中烟工业有限责任公司 | Porous starch-loaded molecular capsule, and preparation method and application thereof |
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2020
- 2020-08-04 CN CN202010771967.5A patent/CN111972423B/en active Active
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| CN102742581A (en) * | 2012-07-20 | 2012-10-24 | 陕西省微生物研究所 | Preparation method of natamycin-hydroxypropyl-beta-cyclodextrin inclusion complex |
| CN105664172A (en) * | 2016-01-19 | 2016-06-15 | 宁夏金太阳药业有限公司 | Preparation method of menthol inclusion compound |
| CN110982620A (en) * | 2019-11-26 | 2020-04-10 | 云南中烟工业有限责任公司 | Porous starch-loaded molecular capsule, and preparation method and application thereof |
Non-Patent Citations (2)
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| 朱平.介孔纳米材料MCM-41搭载两种药物的研究.《中国优秀硕士学位论文全文数据库 医药科技辑》.2019, * |
| 田文军.介孔硅对阿维菌素吸附及释放的形态学效应.《中国优秀硕士学位论文全文数据库 工程科技I辑》.2017, * |
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