CN111606799B - Preparation method and application of medicinal composite vegetable fatty acid magnesium - Google Patents
Preparation method and application of medicinal composite vegetable fatty acid magnesium Download PDFInfo
- Publication number
- CN111606799B CN111606799B CN202010625612.5A CN202010625612A CN111606799B CN 111606799 B CN111606799 B CN 111606799B CN 202010625612 A CN202010625612 A CN 202010625612A CN 111606799 B CN111606799 B CN 111606799B
- Authority
- CN
- China
- Prior art keywords
- magnesium
- mixture
- fatty acid
- stirring
- prepared
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a preparation method of medicinal composite vegetable fatty acid magnesium, which comprises the following steps: s1: adding polyethylene glycol 200 and linolenic acid under the protection of nitrogen, and heating under stirring to obtain a heated mixture A; s2: adding magnesium oxide powder into the mixture A prepared in the step S1, and stirring to prepare a mixture B; s3: heating the mixture B prepared in the step S2 under microwave, adding water and succinic anhydride, keeping the microwave power and temperature unchanged, and increasing the rotating speed to stir for reaction to prepare a reactant; s4: and (5) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, and then introducing water for cooling while stirring to prepare the composite vegetable fatty acid magnesium. The method for producing the medicinal composite vegetable fatty acid magnesium has high efficiency, is suitable for large-scale production, has less environmental pollution, is low-carbon and environment-friendly, and can be widely popularized and applied.
Description
Technical Field
The invention belongs to the technical field of fatty acid magnesium preparation, and particularly relates to a preparation method and application of medicinal composite vegetable fatty acid magnesium.
Background
The magnesium fatty acid is a derivative product of fatty acid, and is widely applied to the fields of high-quality engineering plastic auxiliaries, coating powder, high-grade lubricating grease, medical treatment and the like.
The fatty acid magnesium prepared by the traditional method has excellent performance, but has small magnesium content and can not meet the requirements of popularization and application.
Disclosure of Invention
The invention provides a preparation method and application of medicinal composite vegetable fatty acid magnesium, and aims to solve the problems that fatty acid magnesium prepared by a traditional method is excellent in performance, but has small magnesium content and cannot meet the requirements of popularization and application.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of medicinal composite vegetable fatty acid magnesium comprises the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow during the oxygen discharge, reducing the nitrogen flow after the oxygen discharge is finished, adding polyethylene glycol 200 and linolenic acid under the protection of nitrogen, and heating under stirring to obtain a heated mixture A;
s2: adding magnesium oxide powder into the mixture A prepared in the step S1, and stirring to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 under microwave, adding water and succinic anhydride, keeping the microwave power and temperature unchanged, and increasing the rotating speed to stir for reaction to prepare a reactant;
s4: and (5) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, and then introducing water for cooling while stirring to prepare the composite vegetable fatty acid magnesium.
Preferably, the nitrogen flow is increased to 1-1.4L/min during the oxygen discharge in step S1.
Preferably, the nitrogen flow rate is reduced to 0.1-0.2L/min in step S1.
Preferably, the mass ratio of the polyethylene glycol 200 to the linolenic acid in the step S1 is 25-32: 406-478.
Preferably, the conditions of heating with stirring in step S1: stirring and heating to 60-76 ℃ at the rotation speed of 300-400 r/min.
Preferably, the mass ratio of the magnesium oxide powder to the linolenic acid is 48-60: 406-478.
Preferably, the conditions of stirring in step S2: stirring for 5-8min at the rotation speed of 400-500 r/min.
Preferably, the mixture B prepared in step S2 is heated under microwave in step S3 under the following conditions: the mixture B prepared in the step S2 is heated to 115-123 ℃ under the microwave power of 360-450W.
Preferably, the mass ratio of the water to the succinic anhydride in the step S3 is 40-50: 16-23.
The invention also provides application of the composite vegetable fatty acid magnesium in the field of medicine.
The invention has the following beneficial effects:
(1) the method for preparing the medicinal composite magnesium vegetable fatty acid adopts water cooling, so that the medicinal composite magnesium vegetable fatty acid has good brittleness, is easy to crush to produce powder, not only can greatly reduce the production cost, but also avoids the problem of environmental pollution caused by dust generated by intermittent crushing.
(2) The raw materials are easy to obtain, the price is low, the solvent can be recycled, the prepared medicinal composite vegetable fatty acid magnesium can be used as a novel nontoxic green environment-friendly medicinal product, the magnesium content is up to more than 16.34 percent, the performance is excellent, and the application requirement in the field of medicine can be met.
(3) The method for producing the medicinal composite vegetable fatty acid magnesium has high efficiency, is suitable for large-scale production, has less environmental pollution, is low-carbon and environment-friendly, and can be widely popularized and applied.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
In an embodiment, the preparation method of the medicinal composite vegetable fatty acid magnesium comprises the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow to 1-1.4L/min during the oxygen discharge, reducing the nitrogen flow to 0.1-0.2L/min after the oxygen discharge, adding 25-32g of polyethylene glycol 200 and 478g of linolenic acid under the protection of nitrogen, stirring and heating to 60-76 ℃ at the rotation speed of 300-400r/min to prepare a heated mixture A;
s2: adding 48-60g of magnesium oxide powder into the mixture A prepared in the step S1, and stirring for 5-8min at the rotating speed of 400-500r/min to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 to 115-450W under the microwave power of 360-450W, adding 40-50g of water and 16-23g of succinic anhydride, keeping the microwave power and the temperature unchanged, and increasing the rotation speed to 600-700r/min to stir for 28-32min to prepare a reactant;
s4: and (5) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, and then introducing water for cooling while stirring to prepare the composite vegetable fatty acid magnesium.
The following is a more specific example.
Example 1
A preparation method of medicinal composite vegetable fatty acid magnesium comprises the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow to 1.2L/min during oxygen discharge, reducing the nitrogen flow to 0.1L/min after oxygen discharge, adding 30g of polyethylene glycol 200 and 445g of linolenic acid under the protection of nitrogen, stirring and heating to 72 ℃ at the rotation speed of 400r/min to prepare a heated mixture A;
s2: adding 56g of magnesium oxide powder into the mixture A prepared in the step S1, and stirring for 5min at the rotation speed of 500r/min to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 to 120 ℃ under the microwave power of 450W, adding 46g of water and 20g of succinic anhydride, keeping the microwave power and the temperature unchanged, and increasing the rotating speed to 700r/min to stir and react for 28min to prepare a reactant;
s4: and (4) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, stirring, introducing water, and cooling to prepare the composite magnesium phytofate, wherein the composite magnesium phytofate is applied to the field of medicines.
Example 2
A preparation method of medicinal composite vegetable fatty acid magnesium comprises the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow to 1L/min during oxygen discharge, reducing the nitrogen flow to 0.1L/min after oxygen discharge, adding 26g of polyethylene glycol 200 and 410g of linolenic acid under the protection of nitrogen, stirring and heating at the rotating speed of 300r/min to 62 ℃, and preparing a heated mixture A;
s2: adding 50g of magnesium oxide powder into the mixture A prepared in the step S1, and stirring for 8min at the rotating speed of 400r/min to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 to 116 ℃ under the microwave power of 380W, adding 42g of water and 17g of succinic anhydride, keeping the microwave power and the temperature unchanged, and increasing the rotating speed to 600r/min to stir and react for 32min to prepare a reactant;
s4: and (4) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, stirring, introducing water, and cooling to prepare the composite magnesium phytofate, wherein the composite magnesium phytofate is applied to the field of medicines.
Example 3
A preparation method of medicinal composite vegetable fatty acid magnesium comprises the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow to 1.4L/min during oxygen discharge, reducing the nitrogen flow to 0.1L/min after oxygen discharge, adding 31g of polyethylene glycol 200 and 470g of linolenic acid under the protection of nitrogen, stirring and heating at the rotating speed of 300r/min to 76 ℃ to prepare a heated mixture A;
s2: adding 58g of magnesium oxide powder into the mixture A prepared in the step S1, and stirring for 6min at the rotation speed of 500r/min to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 to 123 ℃ under the microwave power of 420W, adding 50g of water and 22g of succinic anhydride, keeping the microwave power and the temperature unchanged, and increasing the rotating speed to 700r/min to stir and react for 29min to prepare a reactant;
s4: and (4) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, stirring, introducing water, and cooling to prepare the composite magnesium phytofate, wherein the composite magnesium phytofate is applied to the field of medicines.
Comparative example 1
The method for preparing the magnesium salt of medicinal complex plant fatty acid in example 1 was substantially the same, except that polyethylene glycol 200 was not added in step S1.
Comparative example 2
Substantially the same procedure as in example 1 was conducted except that the microwave treatment was not conducted in step S3.
Comparative example 3
The method for preparing the medicinal magnesium complex phytofatty acid in example 1 was substantially the same, except that succinic anhydride was not added in step S3.
The magnesium contents of the fatty acid magnesium prepared in examples 1 to 3 of the present invention and comparative examples 1 to 3 were measured, and the results are shown in the following table.
| Experimental groups | Magnesium content (%) |
| Example 1 | 18.01 |
| Example 2 | 16.34 |
| Example 3 | 17.26 |
| Comparative example 1 | 14.13 |
| Comparative example 2 | 15.98 |
| Comparative example 3 | 15.29 |
From the above table, it can be seen that: (1) as can be seen from the data of examples 1-3, the magnesium content is as high as 16.34% or more, with example 1 being the most preferred example.
(2) From the data of example 1 and comparative example 1, it can be seen that the magnesium content of example 1 is increased 27.46% compared with that of comparative example 1 by adding polyethylene glycol 200, which is that the added polyethylene glycol 200 can sufficiently disperse and emulsify linolenic acid, the particle size of the emulsified linolenic acid is as small as 0.1-46 μm, so as to achieve sufficient reaction with magnesium succinate, and magnesium oxide is excessive, thereby increasing the magnesium content of fatty acid magnesium.
(3) It can be seen from the data of example 1 and comparative example 2 that the microwave treatment reaction is beneficial to increase the magnesium content of the fatty acid magnesium and also shortens the preparation time.
(4) It can be seen from the data of example 1 and comparative example 3 that the magnesium content of example 1 is increased by 17.79% compared with the magnesium content of comparative example 3 after succinic anhydride is added, that is, the added succinic anhydride reacts with water to generate succinic acid, which can catalyze the reaction to allow the magnesium succinate to react with linolenic acid more sufficiently, and magnesium oxide is excessive, so that the magnesium content of fatty acid magnesium is increased.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (8)
1. A preparation method of medicinal composite vegetable fatty acid magnesium is characterized by comprising the following steps:
s1: introducing nitrogen into the reaction kettle for oxygen discharge, increasing the nitrogen flow during oxygen discharge, reducing the nitrogen flow after oxygen discharge, adding polyethylene glycol 200 and linolenic acid under the protection of nitrogen, wherein the mass ratio of the polyethylene glycol 200 to the linolenic acid is 25-32: 406-containing 478, and heating under stirring to obtain a heated mixture A;
s2: adding magnesium oxide powder into the mixture A prepared in the step S1, and stirring to prepare a mixture B;
s3: heating the mixture B prepared in the step S2 under microwave, adding water and succinic anhydride, keeping the microwave power and temperature unchanged, and increasing the rotating speed to stir for reaction to prepare a reactant;
s4: and (5) filtering and dehydrating the reactant prepared in the step (S3), recovering succinic acid and polyethylene glycol 200, and then introducing water for cooling while stirring to prepare the composite vegetable fatty acid magnesium.
2. The method for preparing magnesium fatty acid complex for pharmaceutical use according to claim 1, wherein nitrogen flow is increased to 1-1.4L/min during the oxygen discharge in step S1.
3. The method for preparing magnesium complex phytofatty acid for pharmaceutical use according to claim 1, wherein in step S1, the flow rate of nitrogen is adjusted to 0.1-0.2L/min.
4. The method for preparing magnesium complex phytofatty acid for pharmaceutical use according to claim 1, wherein the heating conditions in step S1 under stirring are: stirring and heating to 60-76 ℃ at the rotation speed of 300-400 r/min.
5. The method for preparing magnesium phytocomplex fatty acid for medical use as claimed in claim 1, wherein the mass ratio of the magnesium oxide powder to the linolenic acid is 48-60: 406-478.
6. The method for preparing magnesium complex phytofatty acid for pharmaceutical use according to claim 1, wherein the stirring conditions in step S2 are as follows: stirring for 5-8min at the rotation speed of 400-500 r/min.
7. The method for preparing magnesium complex phytofatty acid for pharmaceutical use according to claim 1, wherein the conditions of heating mixture B prepared in step S2 under microwave in step S3 are as follows: the mixture B prepared in the step S2 is heated to 115-123 ℃ under the microwave power of 360-450W.
8. The method for preparing magnesium pharmaceutically acceptable complex vegetable fatty acid according to claim 1, wherein the mass ratio of water to succinic anhydride in step S3 is 40-50: 16-23.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010625612.5A CN111606799B (en) | 2020-07-02 | 2020-07-02 | Preparation method and application of medicinal composite vegetable fatty acid magnesium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010625612.5A CN111606799B (en) | 2020-07-02 | 2020-07-02 | Preparation method and application of medicinal composite vegetable fatty acid magnesium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111606799A CN111606799A (en) | 2020-09-01 |
| CN111606799B true CN111606799B (en) | 2021-01-05 |
Family
ID=72198719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010625612.5A Active CN111606799B (en) | 2020-07-02 | 2020-07-02 | Preparation method and application of medicinal composite vegetable fatty acid magnesium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111606799B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112774807B (en) * | 2020-12-31 | 2022-05-31 | 厦门旭翀生物医药科技有限公司 | Preparation method of palm oil fatty acid magnesium |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257882C (en) * | 2004-04-14 | 2006-05-31 | 中国科学院新疆理化技术研究所 | Method for synthesizing edible conjugated calcium linoleic acid |
| US8178707B2 (en) * | 2010-03-25 | 2012-05-15 | Jost Chemical Company | Co-precipitated salts of fatty acids |
| CN104003864A (en) * | 2014-06-09 | 2014-08-27 | 广东信诚达科技有限公司 | Fatty acid alkaline-earth metal salt and preparation method thereof |
| CN105254487A (en) * | 2015-10-23 | 2016-01-20 | 山东广通宝医药有限公司 | Environment-friendly metal carboxylate and preparation method thereof |
-
2020
- 2020-07-02 CN CN202010625612.5A patent/CN111606799B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111606799A (en) | 2020-09-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111606799B (en) | Preparation method and application of medicinal composite vegetable fatty acid magnesium | |
| CN104262493B (en) | A kind of preparation method and purposes of medicinal gel hydroxypropyl starch | |
| CN103755866A (en) | Modified waste oil coating material and application of the same in coating slow/controlled release fertilizers | |
| CN113087873B (en) | Ester exchange type dynamic covalent polymer network material containing non-planar ring and preparation method thereof | |
| CN110452181B (en) | Synthesis method of 2-methyl-4-amino-5-formamide methylpyrimidine | |
| CN102993009B (en) | Preparation method of glycerin monostearate alpha crystal | |
| CN102276348B (en) | Degradable controlled release film and method for producing degradable controlled release film slow release fertilizer | |
| CN111732505B (en) | Preparation method and application of medicinal composite vegetable fatty acid zinc | |
| CN109369757B (en) | Method for preparing Sofosbuvir crystal form 6 | |
| CN111848389A (en) | Preparation method and application of palm oil fatty acid magnesium | |
| CN112850759A (en) | Production process of magnesium oxide | |
| CN113957101A (en) | Method for producing inositol by fermenting recombinant escherichia coli | |
| CN110950838A (en) | Method for synthesizing nicotine salt under solvent-free condition by using microchannel reactor | |
| CN115558090B (en) | Preparation method of polybutylene succinate with low tetrahydrofuran content | |
| CN115073417B (en) | Method for preparing lactide by catalyzing lactic acid with ternary composite catalyst | |
| CN117466810B (en) | Industrial continuous production method of picloram | |
| CN1053664C (en) | Process for producing methaldehyde | |
| CN107973862A (en) | A kind of method that hypoglycemic banana flowers polysaccharide is extracted from banana flowers | |
| CN112679638A (en) | Hydrosolvent polyacrylic resin and preparation method thereof | |
| CN109337053B (en) | Preparation method of polyricinoleate | |
| CN1054618C (en) | Method for preparation of dry power briquetting binder | |
| CN109651456B (en) | Preparation method of sucrose oleate with high monoester content | |
| CN116478039A (en) | Preparation method of medicinal mixed fatty glyceride | |
| CN116332783A (en) | Continuous preparation method of N-ethoxyoxalyl alanine ethyl ester | |
| CN114230456A (en) | Synthesis process of cobalt acetate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |