CN113264822A - Preparation method of disodium fumarate - Google Patents
Preparation method of disodium fumarate Download PDFInfo
- Publication number
- CN113264822A CN113264822A CN202110530646.0A CN202110530646A CN113264822A CN 113264822 A CN113264822 A CN 113264822A CN 202110530646 A CN202110530646 A CN 202110530646A CN 113264822 A CN113264822 A CN 113264822A
- Authority
- CN
- China
- Prior art keywords
- disodium fumarate
- fumaric acid
- drying
- mass
- reaction
- 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.)
- Granted
Links
- MSJMDZAOKORVFC-SEPHDYHBSA-L disodium fumarate Chemical compound [Na+].[Na+].[O-]C(=O)\C=C\C([O-])=O MSJMDZAOKORVFC-SEPHDYHBSA-L 0.000 title claims abstract description 37
- 235000019294 sodium fumarate Nutrition 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims abstract description 58
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001530 fumaric acid Substances 0.000 claims abstract description 29
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000012452 mother liquor Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 239000003960 organic solvent Substances 0.000 abstract description 10
- 238000002425 crystallisation Methods 0.000 abstract description 9
- 230000008025 crystallization Effects 0.000 abstract description 9
- 230000007306 turnover Effects 0.000 abstract description 6
- 238000000967 suction filtration Methods 0.000 abstract description 3
- 241000894006 Bacteria Species 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000011109 contamination Methods 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 2
- 239000010413 mother solution Substances 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 17
- 239000012295 chemical reaction liquid Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000001694 spray drying Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000006260 foam Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004042 decolorization Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000007873 sieving Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical compound [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 description 1
- 239000001744 Sodium fumarate Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011773 ferrous fumarate Substances 0.000 description 1
- 229960000225 ferrous fumarate Drugs 0.000 description 1
- 235000002332 ferrous fumarate Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229940005573 sodium fumarate Drugs 0.000 description 1
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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of compound preparation, and discloses a preparation method of disodium fumarate, which comprises the steps of taking sodium carbonate or sodium hydroxide and fumaric acid as raw materials, taking water as a solvent, reacting at 75-85 ℃, adjusting the pH value of a reaction solution to 6.5-7.5 after the reaction is finished, decoloring, filtering, cooling and crystallizing the reaction solution, extracting a mother solution of a crystallized material, performing solid-liquid separation, starting a discharging device of a vacuum concentrator, discharging the separated material from the vacuum concentrator into a boiling drying pot, and drying to obtain a disodium fumarate product. The method uses a one-step concentration, crystallization and suction filtration device, greatly saves the material turnover time and the risk of contamination of transfer bacteria and foreign matters in the production process, and improves the safety factor of the production environment without using organic solvent; the product has no solvent residue, the water content is easy to control while the product quality is improved, and the method is simple and convenient to operate, low in cost and suitable for popularization and application in the market.
Description
Technical Field
The invention belongs to the technical field of compound preparation, and particularly relates to a preparation method of disodium fumarate.
Background
Disodium fumarate is an important food additive and a medical intermediate, and can be used as a food seasoning, a ferrous fumarate raw material and a biochemical research preparation. At present, no production process report about the product exists, and due to the low yield of the disodium fumarate and the particularity of easy moisture absorption, the inventor tries processes such as concentration, crystallization, drying, spray drying and the like, wherein the concentration, crystallization and drying process needs continuous production due to multiple operation steps and low yield so as to reduce the production cost; the spray drying process has high production cost, high water content of the product and fine granularity of the product, so the use of the spray drying process is influenced.
Therefore, how to provide a preparation method of disodium fumarate, which is simple and convenient in process operation and low in production cost, is a technical problem to be solved urgently by technical personnel in the field.
Disclosure of Invention
In view of the above, the invention aims to solve the technical problems of difficult crystallization, high solubility, low yield and high product quality requirement in the prior art, and adopts a method combining vacuum concentration, crystallization, suction filtration and normal pressure drying to prepare a disodium fumarate product.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of disodium fumarate specifically comprises the following steps:
(1) taking sodium carbonate or sodium hydroxide and fumaric acid as raw materials, taking water as a solvent, reacting at the temperature of 75-85 ℃, adjusting the pH value of a reaction solution to 6.5-7.5 after the reaction is finished, and decoloring, filtering, concentrating and cooling the reaction solution for later use;
(2) cooling and crystallizing the reactant treated in the step (1) in a special vacuum concentrator at the temperature of 25-15 ℃, and maintaining for 2 hours to obtain a crystallized material;
(3) starting a vacuum filtration device of a vacuum concentrator, pumping out the mother liquor of the crystallized materials, and carrying out solid-liquid separation; and then starting a discharging device of the vacuum concentrator, and discharging the separated material from the vacuum concentrator into a boiling drying pot for drying under normal pressure to obtain the disodium fumarate product.
The method disclosed and protected by the invention does not use an organic solvent in the preparation process, so that the safety factor in the production process is reduced, various risks caused by material turnover are blocked, and the disodium fumarate product has no organic solvent residue, so that the quality of the product is improved, the water content is easy to control, and the water content is stable.
In addition, the method disclosed and protected by the invention only uses a one-step concentration crystallizer in the extraction process, does not relate to various reaction equipment, organic solvents and large spray drying equipment, occupies small area and greatly reduces the cost of products.
Preferably, in the step (1), the mass of the fumaric acid is 15-40% of that of the water; the ratio of the amount of fumaric acid to sodium carbonate or sodium hydroxide is 1:1 to 2.
More preferably, in the step (1), the mass of the fumaric acid is 25% of the mass of the water; the mass ratio of fumaric acid to sodium carbonate or sodium hydroxide was 1: 1.
In addition, in the step (1), after the solution is concentrated to 55-65 DEG Be of Baume degree, the temperature of the solution is reduced to 25-15 ℃ for later use.
Preferably, in the step (3), the drying temperature of the materials in the boiling drying pot is 75-85 ℃, and the drying time is 30-45 minutes.
Compared with the prior art, the invention discloses and provides a preparation method of disodium fumarate, which has the advantages that:
(1) the method disclosed and protected by the invention does not use an organic solvent in the preparation process, so that the safety coefficient in the production process is reduced, various risks caused by material turnover are blocked, and the disodium fumarate product has no organic solvent residue, so that the quality of the product is improved, the water content is easy to control, and the water content is stable.
In addition, the method disclosed and protected by the invention only uses a one-step concentration crystallizer in the extraction process, does not relate to various reaction equipment, organic solvents and large spray drying equipment, occupies small area and greatly reduces the cost of products.
(2) The conventional production process of the disodium fumarate is complex in flow and long in production period, the production time of a single-batch product is about 26.5 hours, and the yield is only about 60%; after the preparation process disclosed and protected by the invention is adopted, the turnover of production equipment is reduced, the production time is greatly shortened, the production time of a single-batch product is about 15 hours, and the time is saved by 43.4%; and the solid-liquid ratio of the existing conventional cooling crystallization process is 6: 4, and the solid-to-liquid ratio is 9: 1, the product yield is greatly improved, and the loss is reduced.
Therefore, the analysis is integrated, so that the method provided by the invention uses a one-step concentration, crystallization and suction filtration device, the material turnover time and the risk of contamination of transfer bacteria and foreign matters in the production process are greatly saved, and meanwhile, the safety factor of the production environment is improved without using an organic solvent; the product has no solvent residue, the water content is easy to control while the product quality is improved, and the method is simple and convenient to operate, low in cost and suitable for popularization and application in the market.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
Example 1
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 30% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.5 (the time for feeding the materials for reaction is 3 hours); the reaction solution is decolorized and filtered (2 hours for decolorization and filtration), and then enters a vacuum concentration integral tank to be concentrated until the solid is cooled (5 hours for use), and the water content of the solid is about 8-10%.
(2) Transferring the solid into an oven, drying for 50 minutes at the temperature of 110 ℃, discharging, sieving, bagging and sealing after the moisture is less than or equal to 1 percent to obtain the disodium fumarate product (the use time is 2 hours), wherein the solid yield is 98 percent.
When in total use: 12 hours and 50 minutes
Example 2
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 35% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.7 (the time for feeding the materials for reaction is 3 hours); the reaction solution is decolorized and filtered (2 hours for decolorization and filtration), and then is concentrated in a vacuum concentration integral tank until the solid is cooled (5 hours for use), and the water content of the solid is about 6-8%.
(2) Transferring the solid into a fluidized drying pot, drying at 85 ℃ for 40 minutes until the water content is less than or equal to 1%, discharging, screening, bagging and sealing to obtain the disodium fumarate product (the use time is 2 hours), wherein the solid yield is 99%.
When in total use: 12 hours and 40 minutes
Example 3
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 40% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.7 (the time for feeding the materials for reaction is 3 hours); the reaction solution is decolorized and filtered (2 hours for decolorization and filtration), and then is concentrated in a vacuum concentration integral tank to a solid (5 hours for use), wherein the water content of the solid is about 4-6%.
(2) Transferring the solid into a fluidized drying pot, drying for 30 minutes at the temperature of 85 ℃, discharging, screening, bagging and sealing after the moisture content is less than or equal to 1 percent to obtain the disodium fumarate product (the use time is 2 hours), wherein the solid yield is 98 percent.
When in total use: 12 hours and 30 minutes.
In addition, in order to further illustrate the non-obvious effect of the technical scheme disclosed and protected by the invention compared with the prior art, the inventor also performs the following experiments:
comparative example 1
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 40% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.5 (the time for feeding the materials for reaction is 3 hours); the reaction solution is decolorized and filtered (2 hours are needed for decolorization and filtration), enters a common vacuum concentration tank for concentration (4 hours are needed), and is concentrated to the Baume degree of the solution: 42.5 DEG Be
(2) Transferring the concentrated liquid to a crystallizing tank for cooling and crystallizing (the time is 12 hours), wherein the solid-liquid ratio after crystallization is about 4: 6;
(3) centrifuging the crystallized material in a centrifuge to obtain wet material with water content of about 10% (1 hr);
(4) transferring the solid into a fluidized drying pot, drying for 50 minutes at the temperature of 85 ℃, discharging, sieving, bagging and sealing after the moisture is less than or equal to 1 percent to obtain the disodium fumarate product (the use time is 2 hours), wherein the solid yield is 32 percent.
When in total use: 24 hours and 50 minutes
Comparative example 2
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 45% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.7 (the time for feeding the materials for reaction is 3 hours); and (3) decolorizing and filtering the reaction solution (2 hours for decolorizing and filtering), cooling and crystallizing in a crystallizing tank (12 hours for using), wherein the solid-to-liquid ratio after crystallization is about 1: 4;
(2) putting the crystallized material into a centrifuge for centrifugation to obtain a wet material with the water content of about 10 percent (the time for use is 3 hours);
(3) transferring the solid into a fluidized drying pot, drying for 50 minutes at the temperature of 85 ℃, discharging after the moisture is less than or equal to 1%, discharging, sieving, bagging and sealing to obtain the disodium fumarate product (the use time is 2 hours), wherein the solid yield is 15%.
When in total use: 22 hours and 50 minutes
Comparative example 3
A preparation method of disodium fumarate comprises the following steps:
(1) adding water into a reaction kettle, stirring by a motor, heating to 75 ℃, maintaining stirring, and alternately adding fumaric acid and sodium carbonate according to a mass ratio of 3: 2, alternating for 5 minutes to prevent excessive foam from splashing out of the feed liquid; wherein the mass of the fumaric acid is 40% of the mass of the water, and the mass ratio of the fumaric acid to the sodium carbonate is 1: 1. filtering a small amount of reaction liquid to remove impurities, testing the pH value, and correcting the pH value of the reaction liquid to be 6.7, wherein the reaction time is 3 hours); the reaction solution was decolorized and filtered, and then fed into a storage tank (for 2 hours for decolorization and filtration).
(2) The liquid in the storage tank is directly sprayed and dried by a spray drying device, the inlet air temperature of spray drying is set to be 150 ℃, white powder (60 hours in use) with the water content of 7-9 percent and the granularity of about 300 meshes is obtained, and the solid yield is 98 percent.
When in total use: 65 hours
TABLE 1 quality test results of disodium fumarate products prepared in examples 1-3 and comparative example 3
TABLE 2 comparison of production times and yields of disodium fumarate products prepared in examples 1-3 and comparative examples 1-3
And (4) conclusion: the disodium fumarate prepared in examples 1 to 3 does not use an organic solvent in the preparation process, has less material turnover and high time utilization rate, improves the quality and yield of the product, is easy to control the water content of crystals, and is stable in the water content of the sodium fumarate prepared in examples 1 to 3. Because the concentration and drying use integrated equipment, large-scale equipment of organic solvent and spray drying is not involved, and the cost of products with small occupied area is greatly reduced. And the purity of the disodium fumarate prepared by the method provided by the invention also meets the conventional range: 98.5 to 100 percent.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. The preparation method of disodium fumarate is characterized by comprising the following steps:
(1) taking sodium carbonate or sodium hydroxide and fumaric acid as raw materials, taking water as a solvent, reacting at the temperature of 75-85 ℃, adjusting the pH value of a reaction solution to 6.5-7.5 after the reaction is finished, and decoloring, filtering, concentrating and cooling the reaction solution for later use;
(2) cooling and crystallizing the reactant treated in the step (1) in a special vacuum concentrator at the temperature of 25-15 ℃, and maintaining for 2 hours to obtain a crystallized material;
(3) starting a vacuum filtration device of a vacuum concentrator, pumping out the mother liquor of the crystallized materials, and carrying out solid-liquid separation; and then starting a discharging device of the vacuum concentrator, and discharging the separated material from the vacuum concentrator into a boiling drying pot for drying under normal pressure to obtain the disodium fumarate product.
2. The method for preparing disodium fumarate according to claim 1, wherein in the step (1), the mass of the fumaric acid is 15-40% of that of water; the ratio of the amount of fumaric acid to sodium carbonate or sodium hydroxide is 1:1 to 2.
3. The method for preparing disodium fumarate according to claim 2, wherein in the step (1), the mass of the fumaric acid is 25% of the mass of water; the mass ratio of fumaric acid to sodium carbonate or sodium hydroxide was 1: 1.
4. The method for preparing disodium fumarate according to claim 1 or 2, wherein in the step (1), after the solution is concentrated to 55-65 ° Be, the solution is cooled to 25-15 ℃ for later use.
5. The method for preparing disodium fumarate according to claim 1, wherein in the step (3), the drying temperature of the materials in the boiling drying pot is 75-85 ℃, and the drying time is 30-45 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110530646.0A CN113264822B (en) | 2021-05-15 | 2021-05-15 | Preparation method of disodium fumarate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110530646.0A CN113264822B (en) | 2021-05-15 | 2021-05-15 | Preparation method of disodium fumarate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113264822A true CN113264822A (en) | 2021-08-17 |
| CN113264822B CN113264822B (en) | 2024-04-05 |
Family
ID=77230885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110530646.0A Active CN113264822B (en) | 2021-05-15 | 2021-05-15 | Preparation method of disodium fumarate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113264822B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2848366A (en) * | 1956-05-18 | 1958-08-19 | Mallinckrodt Chemical Works | Non-hydrated ferrous fumarate and hematinic composition thereof |
| CN102370055A (en) * | 2010-08-24 | 2012-03-14 | 北京英惠尔生物技术有限公司 | Preparation method of feeding ferrous fumarate |
| CN107473956A (en) * | 2017-08-29 | 2017-12-15 | 南京雪郎化工科技有限公司 | A kind of production method of ferrous fumarate |
-
2021
- 2021-05-15 CN CN202110530646.0A patent/CN113264822B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2848366A (en) * | 1956-05-18 | 1958-08-19 | Mallinckrodt Chemical Works | Non-hydrated ferrous fumarate and hematinic composition thereof |
| CN102370055A (en) * | 2010-08-24 | 2012-03-14 | 北京英惠尔生物技术有限公司 | Preparation method of feeding ferrous fumarate |
| CN107473956A (en) * | 2017-08-29 | 2017-12-15 | 南京雪郎化工科技有限公司 | A kind of production method of ferrous fumarate |
Non-Patent Citations (2)
| Title |
|---|
| ARIJIT HALDER ET AL: "Structural Diversity in Six Mixed Ligand Zn(II) Meta-Organic Frameworks Constructed by Rigid and Flexible Dicarboxylates and Different N,N’-Donor Ligand", 《CRYSTAL GROWTH ＆ DESIGN》 * |
| 章燕;徐虹;李莎;: "L-天冬氨酸的清洁提取工艺", 生物加工过程 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113264822B (en) | 2024-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6218574B1 (en) | Process for purifying long-chain dicarboxylic acid | |
| CN108358807B (en) | Method and device for recycling and treating acidic DMF (dimethyl formamide) and waste residue sodium acetate | |
| CN102911036A (en) | Method for obtaining high pure dicarboxylic acid | |
| CN105859802B (en) | A kind of crystallization of Sucralose and purification process | |
| CN111087326A (en) | Method for refining guanidine nitrate | |
| CN112552167B (en) | Preparation method of calcium gluconate | |
| WO2021212535A1 (en) | Method for refining benzhexol hydrochloride | |
| CN104355990B (en) | Method for recycling and mechanically using L- (+) -tartaric acid in D-ethyl ester production | |
| CN113264822B (en) | Preparation method of disodium fumarate | |
| CN109503441B (en) | Preparation method of high-content cysteamine hydrochloride | |
| CN109761800B (en) | Method for removing oxalic acid by continuous crystallization in glyoxylic acid production process | |
| WO2023066026A1 (en) | Method for purifying ethylene carbonate by means of dynamic crystallization | |
| CN115231990B (en) | Preparation method of high-purity dipentaerythritol | |
| CN110606863B (en) | Preparation method of N-acetylneuraminic acid dihydrate | |
| CN114292203A (en) | Preparation method of DL-panthenol | |
| CN111138311B (en) | Production method of m-aminoacetanilide | |
| CN114014835A (en) | Glycolide purification process | |
| CN110272451B (en) | Preparation method of tetraphenylphenol phosphonium salt | |
| CN109503325B (en) | Method for reducing chroma of pentaerythritol | |
| EP0421046A1 (en) | Process for producing highly pure 3,3',4,4' - biphenyltetra- carboxylic acid or dianhydride thereof | |
| CN112939032A (en) | Method for preparing potassium nitrate by nitric acid method | |
| CN104326901B (en) | Method for recycling and mechanically using L- (+) -tartaric acid in D-ethyl ester production | |
| CN115626882B (en) | Purification method of creatine monohydrate | |
| CN112979450B (en) | Preparation method of ammonium azelate hydrogen | |
| CN112979451B (en) | Preparation method of ammonium azelate hydrogen |
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 |