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Preparation method of disodium fumarate

A technology of disodium fumarate and fumaric acid, which is applied in the preparation of carboxylate, carboxylate, and organic compounds, etc., which can solve the difficulties of crystallization of disodium fumarate, high product quality requirements, high solubility, etc. problems, to achieve the effect of saving turnover of infectious bacteria and foreign matter, improving product quality, and stabilizing water content

Pending Publication Date: 2021-08-17
吉源(淮北)食品科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, the purpose of the present invention is to prepare disodium fumarate crystallization difficulty in the prior art, the solubility is higher, the yield is lower, the technical problem of high product quality requirement, and adopt vacuum concentration crystallization suction filtration and normal pressure Preparation of Disodium Fumarate Product by Combining Drying Method

Method used

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  • Preparation method of disodium fumarate
  • Preparation method of disodium fumarate

Examples

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Effect test

Embodiment 1

[0024] A preparation method of disodium fumarate, comprising the following steps:

[0025] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, alternately add fumaric acid and sodium carbonate, the mass ratio is about 3:2, and the alternating interval is 5 minutes to prevent excessive foaming The feed liquid is splashed; the mass of fumaric acid is 30% of the mass of water, and the mass ratio of fumaric acid and sodium carbonate is 1:1. Take a small amount of reaction solution to filter and remove impurities, then test the pH, and correct the pH of the reaction solution to 6.5 (3 hours for feeding reaction); decolorize and filter the reaction solution (2 hours for decolorization and filtration), enter the vacuum concentration integrated tank to concentrate to solid cooling (time for reaction) 5 hours), at this moment the solid water content is about 8-10%.

[0026] (2) Transfer the solid to an oven, and dry it for...

Embodiment 2

[0029] A preparation method of disodium fumarate, comprising the following steps:

[0030] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, alternately add fumaric acid and sodium carbonate, the mass ratio is about 3:2, and the alternating interval is 5 minutes to prevent excessive foaming The feed liquid is splashed; the mass of fumaric acid is 35% of the mass of water, and the mass ratio of fumaric acid and sodium carbonate is 1:1. Take a small amount of reaction solution to filter and remove impurities, then test the pH, and correct the pH of the reaction solution to 6.7 (3 hours for feeding reaction); decolorize and filter the reaction solution (2 hours for decolorization and filtration), enter the vacuum concentration integrated tank to concentrate to solid cooling (time for decolorization) 5 hours), at this moment the solid water content is about 6-8%.

[0031] (2) Transfer the solid to the boiling drying...

Embodiment 3

[0034] A preparation method of disodium fumarate, comprising the following steps:

[0035] (1) Add water to the reaction kettle, equipped with a motor to stir, heat to a temperature of 75°C, keep stirring, alternately add fumaric acid and sodium carbonate, the mass ratio is about 3:2, and the alternating interval is 5 minutes to prevent excessive foaming The feed liquid is splashed; the mass of fumaric acid is 40% of the mass of water, and the mass ratio of fumaric acid and sodium carbonate is 1:1. Take a small amount of reaction solution to filter and remove impurities, then test the pH, and correct the pH of the reaction solution to 6.7 (3 hours for feeding reaction); decolorize and filter the reaction solution (2 hours for decolorization and filtration), enter the vacuum concentration integrated tank to concentrate to solid (5 hours for the reaction). hours), at this time the solid moisture content is about 4-6%.

[0036] (2) Transfer the solid to the boiling drying pot, d...

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Abstract

The invention relates to the technical field of compound preparation, and discloses and provides a preparation method of disodium fumarate, which comprises the following steps: by taking sodium carbonate or sodium hydroxide and fumaric acid as raw materials and water as a solvent, reacting at the temperature of 75-85 DEG C, adjusting the pH value of the reaction solution to 6.5-7.5 after the reaction is finished, and then decolorizing, filtering, cooling and crystallizing the reaction solution; and extracting mother liquor of the crystallized material, carrying out solid-liquid separation, starting a discharging device of the vacuum concentrator, discharging the separated material from the vacuum concentrator into a boiling drying pot, and drying to obtain a disodium fumarate product. According to the method, a one-step concentrating, crystallization and suction filtrating device is used, the material turnover time in the production process is greatly shortened, the risk of turnover contamination and foreign matter mixing is greatly reduced, meanwhile, no organic solvent is used, and the safety coefficient of the production environment is increased; and 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 market popularization and application.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of disodium fumarate. Background technique [0002] Disodium fumarate is an important food additive and pharmaceutical intermediate, which can be used as food seasoning, ferrous fumarate raw material and biochemical research preparation. At present, there is no report on the production process of this product, and due to the low yield of disodium fumarate and the particularity of easy moisture absorption, the inventor has tried processes such as concentrated crystallization drying and spray drying. Many steps and low yield require continuous production in order to reduce production costs; while the spray drying process affects the use due to high production costs, high water content of the product, and fine particle size of the product. [0003] Therefore, how to provide a disodium fumarate preparation method with simple process oper...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C51/42C07C51/43C07C57/15
CPCC07C51/412C07C51/42C07C51/43C07C57/15
Inventor 陈沁张玉武林
Owner 吉源(淮北)食品科技有限公司
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