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Production method of high-purity dimethyl fumarate

A technology of dimethyl fumarate and its production method, which is applied in the field of chemistry and chemical engineering, can solve problems such as unresolved production cost and quality problems, high cost of ionic liquids, and no economic advantages, etc., so as to reduce recrystallization steps and reduce costs The effect of large range and high safety in use

Inactive Publication Date: 2014-06-11
徐晓宁
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In CN102432464A, fumaric acid reacts with 6 to 10 times of methanol in cationic resin catalysts. Although continuous operation is achieved, steps such as secondary filtration, neutralization, and washing are added to obtain dimethyl fumarate. greatly surpasses the invention
[0009] In CN102757346A, the ionic liquid catalyst is used to solve the problem of catalyst recovery, but the production cost and quality problems cannot be solved by adopting batch production. The cost of the ionic liquid of this technology is very expensive, and compared with the previous technology, there is no economic advantage

Method used

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  • Production method of high-purity dimethyl fumarate

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Effect test

Embodiment 1

[0035] to 2m 3 In the enamel reactor, put 500 kg of industrial methanol, 50 kg of 98% concentrated sulfuric acid, and 500 kg of dried industrial waste fumaric acid in sequence, and then pass steam into the jacket to raise the temperature to 50 °C, start stirring, continue Raise the temperature to 90°C, add 1,000 kg of methanol dropwise, and produce through the condenser at the same time. The output enters the jacketed crystallizer, cools and crystallizes, and is filtered and dried by a centrifuge to obtain 158 kg of the product, which has a purity of 99.65 after chemical analysis. %. The calculated yield is: 25.44%.

Embodiment 2

[0037] Add 500 kg of dried industrial waste fumaric acid to the reactor of Example 1. Maintain 90-110°C. According to the method of Example 1., add 5000 kg of methanol dropwise to obtain 356 kg of product. The calculated yield is: 57.34%.

Embodiment 3

[0039] In the reactor of embodiment 2., drop into 500 kilograms of industrial waste fumaric acid through drying again, maintain 90~110 ℃, according to the method for embodiment 1., drop in 5000 kilograms of methanol, including 1000 kilograms of new methanol and 4000 kilograms of methanol are reclaimed to obtain 587 kilograms of product. The calculated yield is: 94.54%.

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Abstract

The invention belongs to the technical field of the chemical industry and discloses a production method of high-purity dimethyl fumarate. The production method is characterized in that during a production process, synthesis and refining processes are finished by one step in an esterification reactor. During a refining reaction process, industrial waste fumaric acid can be taken as a raw material to react with methanol in the presence of a catalyst and a refining process is also finished during the reaction. After the methanol and the catalyst are added into the reactor, the industrial waste fumaric acid is added for reaction, subsequently the methanol and methanol mixed gas which is used for continuously generating the dimethyl fumarate are continuously added and then a high-purity dimethyl fumarate finished product can be obtained after condensation, crystallization, filtration and drying. The production method disclosed by the invention has the advantages of short technological process and high product purity, greatly lowering the cost in comparison with the existing method, and being economic and more reasonable.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a production method of high-purity dimethyl fumarate. Background technique [0002] Dimethyl fumarate is a new type of low-toxicity and high-efficiency preservative newly developed in the 1980s. It has broad-spectrum and high-efficiency characteristics, and has a good inhibitory effect on more than 30 kinds of molds, yeasts and bacteria. Its toxicity is very low (LD50=2240mg / Kg), and after entering the human body, it will quickly become fumaric acid, a normal metabolic component of the human body, so it is extremely safe. It has strong biological activity and is sublimable, so it has dual functions of contact sterilization and fumigation sterilization, which is a rare characteristic of general preservatives. It has good heat resistance and a wide range of pH values, and can be used within the range of pH 3-8. Compared with traditional food preservativ...

Claims

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Application Information

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IPC IPC(8): C07C69/60C07C67/08
CPCC07C67/08C07C69/60
Inventor 徐晓宁赵宝超刘宏羽赵岩
Owner 徐晓宁
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