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Continuous production process for dimethyl fumarate

A technology of dimethyl fumarate and production process, which is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve problems such as low yield and complicated operation, and achieve non-corrosion reaction equipment. , the reaction conditions are simple, the effect of not polluting the environment

Inactive Publication Date: 2012-05-02
费近峰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, many scholars at home and abroad are developing and researching some non-toxic, non-corrosive, and separable solid acid catalysts to replace traditional catalysts. Catalyzed synthesis of fumaric acid such as reports, but the operation is complicated and the yield is not high

Method used

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  • Continuous production process for dimethyl fumarate
  • Continuous production process for dimethyl fumarate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of continuous production process of dimethyl fumarate, such as figure 1 As shown, the 732-type polystyrene sulfonic acid cation exchange resin (purchased from Shanghai Yige Industrial Co., Ltd.) was evenly filled into the reaction column 4 and heated to 70-75 °C; Raw material fumaric acid and methanol solution, the molar ratio is: 1:5, through the feed pump 2, from the feed port 3 of the fixed reaction column into the reaction column 4, adjust the flow rate of the flow pump, control the feed rate of raw materials, Make the residence time of raw material in reaction column be 4h, discharge port 6 collects reaction product; Pass reaction product into cold water, stir, have a large amount of white crystals to separate out; Filter, filter cake with 8%Na 2 CO 3 The solution was washed; filtered again, the filter cake was washed with distilled water until neutral, and then dried at room temperature to obtain the product. The yield was 89.6%.

Embodiment 2

[0020] A kind of continuous production process of dimethyl fumarate, such as figure 1 As shown, the D-61 polystyrene sulfonic acid cation exchange resin (purchased from Shanghai Yige Industrial Co., Ltd.) was evenly filled into the reaction column 4 and heated to 75-80 °C; The reaction raw materials fumaric acid and methanol solution, molar ratio is: 1:8, join in the reaction column 4 from the inlet 3 of fixed reaction column, adjust the flow rate of flow pump, control the addition speed of raw material, make raw material in reaction The residence time in the column is 8h, and the reaction product is collected at 6 outlets; the reaction product is passed into cold water, stirred, and a large amount of white crystals are precipitated; filtered, and the filter cake is washed with 9%Na 2 CO 3 The solution was washed; filtered again, the filter cake was washed with distilled water until neutral, and then dried at room temperature to obtain the product. The yield was 94.3%.

Embodiment 3

[0022] A continuous production process for dimethyl fumarate, D-72 type polystyrene sulfonic acid type cation exchange resin (purchased from Shanghai Yige Industrial Co., Ltd.), is evenly filled in the reaction column 4, heated to 82- 88°C; put the reaction raw material fumaric acid and methanol solution in the raw material cylinder 1, the molar ratio is: 1:6, add it to the reaction column from the feed port 3 of the fixed reaction column, adjust the flow rate of the flow pump, and control The adding speed of raw material makes the residence time of raw material in reaction column be 6h, and the reaction product is collected at 6 places of outlet; Pass reaction product into cold water, stir, have a large amount of white crystals to separate out; Filter, filter cake with 10% Na 2 CO 3 The solution was washed; filtered again, the filter cake was washed with distilled water until neutral, and then dried at room temperature to obtain the product. The yield was 95.7%.

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Abstract

The invention discloses a continuous production process for dimethyl fumarate. The process comprises the following steps of: uniformly filling a strong acid cation exchange resin catalyst into a reaction cylinder, and heating at the temperature of between 60 and 100 DEG C; adding fumaric acid and a methanol solution which serve as reaction raw materials into the reaction cylinder from an inlet of the fixed reaction cylinder, regulating the flow velocity of a flow pump to ensure that the raw materials are kept in the reaction cylinder for 4 to 8 hours, and collecting a reaction product at an outlet; introducing the reaction product into cold water, stirring, and crystallizing a large number of white crystals; filtering, and washing a filter cake by using 8 to 10 percent Na2CO3; and filtering again, washing the filter cake to be neutral by using distilled water, drying at room temperature, and thus obtaining the dimethyl fumarate. In the process, strong acid cation exchange resin is utilized, does not corrode reaction equipment and pollute the environment, can be repeatedly used and is a good environment-friendly catalyst. The catalyst is fixed in the reaction cylinder; the materials are continuously fed and discharged, so that the continuous operation of the reaction can be realized; and the process has simple reaction conditions and makes the operation convenient.

Description

technical field [0001] The invention relates to a continuous production process of dimethyl fumarate. Background technique [0002] Dimethyl fumarate is referred to as DMF, the scientific name is dimethyl fumarate, and the common name is dimethyl fumarate. It is an excellent antiseptic and preservative developed in the 1980s. The deficiencies of hydroxybenzoate, sorbic acid, etc., have the characteristics of broad spectrum, high efficiency, low toxicity, economical and practical, have special inhibitory effect on many molds, and have antifungal ability. Dimethyl fumarate can be widely used in food, vegetables, fruit preservation, antisepsis and insecticide, and can also be used in leather, cosmetics, textiles, pharmaceuticals and other industries, and is constantly developing new application fields. It is a very useful Promising new preservatives have attracted great attention from food and feed industries at home and abroad. The U.S. Food and Drug Administration listed di...

Claims

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Application Information

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IPC IPC(8): C07C69/60C07C67/08
Inventor 费近峰
Owner 费近峰
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