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Process for preparing monomethyl fumarate

A technology of monomethyl fumarate and monomethyl maleate, applied in the technical field of preparing monomethyl fumarate, can solve the problem that the yield of monomethyl fumarate is only 70-80%, and achieve Good environmental performance

Inactive Publication Date: 2002-08-14
CHONGQING MINTAI NEW AGROTECH DEV GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

" Maleic anhydride Methanol monomethyl maleate Monomethyl fumarate In the above process line, due to the selection and improper control of process parameters, the yield of monomethyl fumarate is only 70-80%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: Maleic anhydride and methyl alcohol are dropped in the reaction tank by the ratio (weight ratio) of 98: 32, keep stirring with 45 rev / mins, and reaction system begins to drop in temperature, and this is because maleic anhydride is soluble in methanol Due to physical heat absorption. However, when part of the maleic anhydride dissolves, it will immediately undergo esterification reaction with methanol, and the temperature of the reaction system will start to rise. When the temperature rises to 50°C, cool the reaction tank with cooling water to keep the reaction temperature at 30-70°C After 3 hours, it was cooled to room temperature to obtain monomethyl maleate.

Embodiment 2

[0017] Embodiment 2: Place the monomethyl maleate obtained by the reaction in an isomerization container, add 0.5% concentrated hydrochloric acid of the amount of monomethyl fumarate, mix well, and place in a container that can be air-cooled or water-cooled , keep the temperature of the whole isomerization reaction system at 60°C. After standing still for 50 hours, the monomethyl fumarate was taken out, and the powdery monomethyl fumarate product was obtained after crushing, with a yield of not less than 95%.

Embodiment 3

[0018] Embodiment 3: Solvent isomerization: the monomethyl maleate obtained by the reaction is placed in a reaction pot, ethyl acetate is added, the ratio of monomethyl maleate to ethyl acetate is 1: 3, then maleic acid is added The concentrated hydrochloric acid of 1% of monomethyl ester weight, keep 50 rev / min stirring, finish after 6 hours. During the isomerization process, cooling water is used to control the isomerization reaction temperature at about 50°C. Most of the monomethyl fumarate precipitates out in the form of precipitation, and it is centrifuged (3000 rpm) for 7 minutes to obtain monomethyl fumarate, which contains about 5-8% ethyl acetate, and placed at 50°C In the left and right ovens, the pure product of monomethyl fumarate was obtained after vacuum drying for 1 hour. This method is more complicated than the direct isomerization method. But because solvent exists in the isomerization process, the reaction temperature is easy to control, the product purity i...

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Abstract

A process for preparing monomethyl fumarate from maleic acid anhydride as raw material includes such steps as alcoholizing by methanol at 30-70 deg.C for 1.5-5 hr while stirring, adding concentrated hydrochloric acid and isomerizing reaction at 30-80 deg.C for 20-60 hr (or adding ethyl acetate and then concentrated hydrochloric acid and isomerizing at 20-70 deg.C for 3-8 hr while stirring), centrifugal separation and vacuum drying. Its advantages include high output rate (95%), very low energy consumption and no environmental pollution.

Description

(1) Technical field [0001] The invention relates to a preparation process of an antiseptic, in particular to a preparation process of monomethyl fumarate. (2) Technical background [0002] At present, in the preservative industry, dimethyl fumarate (DMF) is widely used due to its excellent anti-mold effect, but DMF is severely irritating to the skin and eyes, and can cause skin allergies when it comes into contact with the human body, especially when used in large amounts The performance is more prominent in summer and autumn. Due to the use of concentrated sulfuric acid in the process, the depreciation of equipment is fast, and waste liquid is generated, which needs to be treated in an environmentally friendly manner. Therefore, people began to pay attention to a preservative with good effect and less irritation—monomethyl fumarate (MMF). MMF not only has the advantages of DMF, such as a wide range of PH applications, low toxicity, high efficiency, wide application, and co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/30C07C69/60
Inventor 洪晓圣陶友能杨梅
Owner CHONGQING MINTAI NEW AGROTECH DEV GRP CO LTD
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