CN111604013A - Method for realizing essence slow release by using polyethylene glycol long-chain alkylamide - Google Patents
Method for realizing essence slow release by using polyethylene glycol long-chain alkylamide Download PDFInfo
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- CN111604013A CN111604013A CN202010269971.1A CN202010269971A CN111604013A CN 111604013 A CN111604013 A CN 111604013A CN 202010269971 A CN202010269971 A CN 202010269971A CN 111604013 A CN111604013 A CN 111604013A
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- Prior art keywords
- polyethylene glycol
- essence
- chain
- glycol long
- slow release
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
- C08G65/325—Polymers modified by chemical after-treatment with inorganic compounds containing nitrogen
- C08G65/3255—Ammonia
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
Abstract
The invention discloses a method for realizing essence slow release by using polyethylene glycol long-chain alkylamide, which specifically comprises the following steps: mixing essence and polyethylene glycol long-chain alkylamide according to a certain proportion, raising the temperature to 40-60 ℃, vigorously stirring for 1 hour, stopping stirring, cooling to below 20 ℃, and separating out solid microspheres to form the essence coated by the polyethylene glycol long-chain alkylamide; the perfume molecules are wrapped by the polyethylene glycol long-chain alkyl amide, so that physical limitation is formed on the perfume molecules, the volatilization speed of the perfume molecules is reduced, and the slow release effect is achieved. The essence solid microspheres coated by the polyethylene glycol long-chain alkyl amide prepared by the two steps can be directly used as a flavoring agent, and can also be added into other products such as perfume, perfume ball and the like instead of pure essence, so that the effects of less essence consumption and more lasting fragrance can be achieved.
Description
Technical Field
The invention relates to the technical field of daily chemicals, cosmetics, essences and spices, in particular to a method for realizing essence slow release by using polyethylene glycol long-chain alkylamide.
Background
Along with the improvement of living standard of people, the use of the essence and the spice is more and more extensive. In addition to traditional perfumes, skin care products, cleaning products, etc., perfumes and fragrances are also used in various automobiles, interiors, and plastic products. The traditional method of using essence is to add a certain amount of essence directly into the relevant product, and then to mix simply. The product prepared by the method has no physical restraint on the perfume molecules, the volatilization speed of the perfume molecules is mainly determined by the ambient temperature and air pressure, and the perfume can disappear quickly under normal conditions, namely the utilization rate of the perfume is low.
Disclosure of Invention
The invention aims to provide a method for realizing essence slow release by using polyethylene glycol long-chain alkylamide aiming at the defects of the prior art, and solves the problems that the fragrance of the existing perfume disappears quickly and the utilization rate of the perfume is low.
The technical scheme for solving the problems comprises the following steps: a method for realizing essence slow release by using polyethylene glycol long-chain alkylamide specifically comprises the following steps: mixing essence and polyethylene glycol long-chain alkylamide according to a certain proportion, raising the temperature to 40-60 ℃, vigorously stirring for 1 hour, stopping stirring, cooling to below 20 ℃, and separating out solid microspheres to form the essence coated by the polyethylene glycol long-chain alkylamide;
the mass ratio of the essence to the polyethylene glycol long-chain alkylamide is 1: 2-4, preferably 1: 3;
the temperature during heating is preferably 50 ℃;
the temperature during temperature reduction is preferably 10 ℃;
the polyethylene glycol long-chain alkylamide has the following structural characteristics:
in the structure, the Alkyl is selected from straight-chain or branched-chain Alkyl containing 6-30 carbons; n is the number of the repeated ethoxy units, namely the corresponding polyethylene glycol fragments with different molecular weights, and the polyethylene glycol fragments are selected from one or more mixtures of polyethylene glycols with the molecular weights of 200-1000, preferably from one or more mixtures of polyethylene glycols with the molecular weights of 200, 300, 400, 500, 600, 800 and 1000.
The invention has the following beneficial effects:
the invention provides a method for realizing essence slow release by using polyethylene glycol long-chain alkyl amide, which utilizes the polyethylene glycol long-chain alkyl amide to wrap spice molecules and forms a physical limit on the spice molecules, thereby reducing the volatilization speed of the spice molecules and achieving the effect of slow release. The essence solid microspheres coated by the polyethylene glycol long-chain alkyl amide prepared by the two steps can be directly used as a flavoring agent, and can also be added into other products such as perfume, perfume ball and the like instead of pure essence, so that the effects of less essence consumption and more lasting fragrance can be achieved.
Detailed Description
In a first step, a polyethylene glycol long chain alkylamide (polyethylene glycol 1000 octadecylamide) is prepared: 100 g (0.1mol) of polyethylene glycol monomethyl ether (mPEG1000) having a molecular weight of 1000, 3 g (0.05mol) of silica and 10 g (0.1mol) of alumina were sequentially added to a 500ml autoclave, ammonia gas was introduced and the pressure was adjusted to 2 atmospheres, and after 36 hours of reaction at 180 ℃, the mixture was extracted three times with water and ethyl acetate to remove the water layer, and the organic layer was dried over anhydrous sodium sulfate. Removing solvent with rotary evaporator, extracting product with dichloromethane, and evaporating to remove solvent to obtain 87 g of polyethylene glycol amine monomethyl ether with yield of 87%, repeating for several times to obtain enough polyethylene glycol amine monomethyl ether (mPEG NH 2);
100 g (0.1mol) of the polyethylene glycol amine monomethyl ether (mPEG NH2) prepared as above and 28 g (0.1mol) of methyl octadecanoate are sequentially added into a 500ml high-pressure reaction kettle, and after the reaction is carried out for 36 hours at 160 ℃, volatile matters are removed by a rotary evaporator to obtain 101 g of polyethylene glycol 1000 octadecyl amide, the yield is 81%, and the reaction is repeated for a plurality of times to obtain enough polyethylene glycol 1000 octadecyl amide.
Second, preparing polyethylene glycol long-chain alkylamide (polyethylene glycol 800 dodecylamide): in a 500ml autoclave, 80 g (0.1mol) of polyethylene glycol monomethyl ether (mPEG800) having a molecular weight of 800, 3 g (0.05mol) of silica and 10 g (0.1mol) of alumina were sequentially charged, ammonia gas was introduced and the pressure was adjusted to 2 atmospheres, and after reacting at 180 ℃ for 36 hours, extraction was carried out three times with water and ethyl acetate to remove the water layer, and the organic layer was dried over anhydrous sodium sulfate. Removing the solvent by using a rotary evaporator, extracting a product by using dichloromethane, and then evaporating the solvent to obtain 67 g of polyethylene glycol amine monomethyl ether, wherein the yield is 84%, and repeating the steps for multiple times to obtain sufficient polyethylene glycol amine monomethyl ether;
80 g (0.1mol) of the polyethylene glycol amine monomethyl ether (mPEG NH2) prepared in the above way and 24 g (0.1mol) of methyl dodecanoate are sequentially added into a 500ml high-pressure reaction kettle, and after the reaction is carried out for 36 hours at 160 ℃, volatile matters are removed by a rotary evaporator to obtain 82 g of polyethylene glycol 800 dodecylamide, the yield is 82%, and the steps are repeated for a plurality of times to obtain enough polyethylene glycol 800 dodecylamide.
Example 1:
mixing 1 kg of citrus essential oil and 3 kg of polyethylene glycol 1000 octadecyl amide prepared in the first step in a container, heating to 50 ℃, then stirring vigorously for 1 hour, stopping stirring, cooling to 10 ℃, and separating out solid microspheres to obtain the citrus flavoring agent coated with polyethylene glycol long-chain alkyl amide, wherein the total amount is about 4 kg.
Example 2:
mixing 1 kg of apple-flavored plant essential oil and 3 kg of polyethylene glycol 1000 octadecyl amide prepared in the first step in a container, heating to 50 ℃, then stirring vigorously for 1 hour, stopping stirring, cooling to 10 ℃, and separating out solid microspheres to obtain the apple flavoring agent coated with polyethylene glycol long-chain alkyl amide, wherein the total amount is about 4 kg.
Example 3:
and (3) mixing 1 kg of rose plant essential oil and 3 kg of polyethylene glycol 800 dodecyl amide prepared in the second step in a container, heating to 50 ℃, then stirring vigorously for 1 hour, stopping stirring, cooling to 10 ℃, and separating out solid microspheres to obtain the rose fragrance type flavoring agent wrapped by the polyethylene glycol 800 dodecyl amide, wherein the total amount is about 4 kg.
Example 4:
and (3) mixing 1 kg of methyl laurate and 3 kg of polyethylene glycol 800 dodecyl amide prepared in the second step in a container, heating to 50 ℃, then stirring vigorously for 1 hour, stopping stirring, cooling to 10 ℃, and separating out solid microspheres to obtain the polyethylene glycol 800 dodecyl amide-coated methyl laurate spice, wherein the total amount is about 4 kg.
Comparative example 1:
with respect to a glycerin solution of methyl laurate in an amount of 80% as a control, 1 g of methyl laurate and 3 g of glycerin were mixed to prepare a glycerin solution of methyl laurate in an amount of 25% as a control.
The samples of example 4 and comparative example 1 were exposed to normal temperature and pressure, and the remaining concentration of methyl laurate in each sample was measured every 10 days. The relative residual ratio is calculated according to the following formula:
relative residual ratio residual methyl laurate concentration/initial methyl laurate concentration;
the final test results were as follows:
| 10 days | 20 days | 30 days | 40 days | 50 days | 60 days | 70 days | 80 days | 90 days | |
| Comparative example 1 | 57％ | 33％ | 21％ | 16％ | 11％ | 9％ | 8％ | 7％ | 6％ |
| Example 4 | 93％ | 87％ | 82％ | 77％ | 73％ | 69％ | 65％ | 64％ | 63％ |
As can be seen from the above table, the volatilization speed of methyl laurate in the polyethylene glycol 800 dodecylamide coated methyl laurate perfume prepared in the sixth embodiment is significantly lower than that of the control group, which fully proves that the perfume slow release technology provided by the present invention can effectively reduce the volatilization speed of the perfume, and achieve the slow release effect.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (7)
1. A method for realizing essence slow release by using polyethylene glycol long-chain alkylamide is characterized in that: the method specifically comprises the following steps: after the essence and the polyethylene glycol long-chain alkyl amide are mixed according to a certain proportion, the temperature is raised to 40-60 ℃, the mixture is stirred vigorously for 1 hour, then the stirring is stopped, the temperature is reduced to below 20 ℃, solid microspheres are separated out, and the essence wrapped by the polyethylene glycol long-chain alkyl amide is formed.
2. The method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the essence to the polyethylene glycol long-chain alkylamide is 1: 2 to 4.
3. The method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 2, characterized in that: the mass ratio of the essence to the polyethylene glycol long-chain alkylamide is 1: 3.
4. the method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 1, wherein the method comprises the following steps: the temperature at the time of temperature rise was 50 ℃.
5. The method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 1, wherein the method comprises the following steps: the temperature during cooling is 10 ℃.
6. The method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 1, wherein the method comprises the following steps: the polyethylene glycol long-chain alkylamide has the following structural characteristics:
in the structure, the Alkyl is selected from straight-chain or branched-chain Alkyl containing 6-30 carbons; n refers to the number of the repeated ethoxy units, namely the corresponding polyethylene glycol fragments with different molecular weights, and the polyethylene glycol fragments are selected from one or a mixture of polyethylene glycol with the molecular weight of 200-1000.
7. The method for realizing essence slow release by using polyethylene glycol long-chain alkylamide as claimed in claim 6, wherein: the polyethylene glycol fragment is selected from one or more of molecular weight 200, 300, 400, 500, 600, 800 and 1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010269971.1A CN111604013A (en) | 2020-04-08 | 2020-04-08 | Method for realizing essence slow release by using polyethylene glycol long-chain alkylamide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010269971.1A CN111604013A (en) | 2020-04-08 | 2020-04-08 | Method for realizing essence slow release by using polyethylene glycol long-chain alkylamide |
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| CN111604013A true CN111604013A (en) | 2020-09-01 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5456916A (en) * | 1990-05-22 | 1995-10-10 | Nippon Kayaku Kabushiki Kaisha | Microcapsules containing capsaicine compound and their production |
| CN1237478A (en) * | 1998-03-05 | 1999-12-08 | 住友化学工业株式会社 | Method for microencapsulating of solid substance |
| CN101412946A (en) * | 2007-10-15 | 2009-04-22 | 深圳波顿香料有限公司 | Nano essence dispersion and preparation thereof |
| CN101513271A (en) * | 2008-12-30 | 2009-08-26 | 无锡华馨香精香料有限公司 | Instant dispersion capsule of tobacco flavor and preparation method thereof |
| WO2012116014A1 (en) * | 2011-02-25 | 2012-08-30 | Milliken & Company | Capsules and compositions comprising the same |
| CN104293486A (en) * | 2013-07-19 | 2015-01-21 | 中国科学院过程工程研究所 | Microencapsulated daily use essence and preparation method thereof |
| US20190233770A1 (en) * | 2016-09-19 | 2019-08-01 | Givaudan Sa | Improvements in or relating to organic compounds |
-
2020
- 2020-04-08 CN CN202010269971.1A patent/CN111604013A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5456916A (en) * | 1990-05-22 | 1995-10-10 | Nippon Kayaku Kabushiki Kaisha | Microcapsules containing capsaicine compound and their production |
| CN1237478A (en) * | 1998-03-05 | 1999-12-08 | 住友化学工业株式会社 | Method for microencapsulating of solid substance |
| CN101412946A (en) * | 2007-10-15 | 2009-04-22 | 深圳波顿香料有限公司 | Nano essence dispersion and preparation thereof |
| CN101513271A (en) * | 2008-12-30 | 2009-08-26 | 无锡华馨香精香料有限公司 | Instant dispersion capsule of tobacco flavor and preparation method thereof |
| WO2012116014A1 (en) * | 2011-02-25 | 2012-08-30 | Milliken & Company | Capsules and compositions comprising the same |
| CN104293486A (en) * | 2013-07-19 | 2015-01-21 | 中国科学院过程工程研究所 | Microencapsulated daily use essence and preparation method thereof |
| US20190233770A1 (en) * | 2016-09-19 | 2019-08-01 | Givaudan Sa | Improvements in or relating to organic compounds |
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Application publication date: 20200901 |