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Continuous synthesis method of dimethyl acetylsuccinate

A technology for the synthesis of dimethyl acetylsuccinate, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of long reaction cycle, low purity of crude products, and insufficient content of final products. To 99% and other problems, to achieve the effect of short reaction cycle and simple process

Inactive Publication Date: 2012-01-11
河北彩客新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of above-mentioned synthetic method is: long reaction cycle (300min), transformation rate is unsatisfactory (90-92%), and crude product purity is low, and final product content can't reach 99%

Method used

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  • Continuous synthesis method of dimethyl acetylsuccinate
  • Continuous synthesis method of dimethyl acetylsuccinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] This reaction is carried out in a stainless steel high-pressure reactor, which is equipped with a temperature control device and a temperature measuring device for heating and cooling devices, an electromagnetic stirring device, a pressure measuring device, a high-pressure continuous discharge device, and a liquid in and out valves, and a high-pressure syringe pump.

[0018] The batching container is placed under an ice-water bath, sequentially add 1000 g of dimethyl maleate, 1220 g of acetaldehyde, and 22 g of benzoyl peroxide, stir to dissolve, and set aside. Add 300ml of the prepared solution into a 500ml stainless steel high-pressure reactor, and close the reactor; stir and heat up, and react at 125°C for 120 minutes, then use a high-pressure syringe pump to continuously feed materials into the reactor at a speed of 12.5ml / min, and open the outlet at the same time. The material is discharged at the same speed. During the reaction, the reaction temperature is control...

Embodiment 2

[0021] Azobisisobutyronitrile was used instead of benzoyl peroxide, and other conditions were the same as in Example 1. The reaction liquid gas chromatography analysis conversion rate was 95.1%, and the gas chromatography analysis content of the crystalline product was 99.17%.

Embodiment 3

[0023] A high-pressure syringe pump feeds into the reactor at a speed of 15 ml / min. Other conditions are the same as in Example 1. The reaction liquid gas chromatography analysis conversion rate is 93.64%, and the crystallization product gas chromatography analysis content is 98.88%.

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Abstract

The invention discloses a continuous synthesis method of dimethyl acetylsuccinate, which comprises the following steps of: continuously pouring dimethyl maleate and acetaldehyde as raw materials into a high-pressure reactor for reaction in the presence of a radical initiator by using a high-pressure pump, continuously blanking reaction liquid, and finally obtaining the dimethyl acetylsuccinate. The method has the advantages of short reaction period, 95% or higher of conversion rate and 99% or higher of product purity. The dimethyl acetylsuccinate is the key intermediate for preparing novel environment-friendly food colors, such as dimethyl acetylsuccinate ketone carboxylate, namely lemon yellow, and the like.

Description

technical field [0001] The invention belongs to chemical industry synthesis technology, in particular to a synthesis method of dimethyl acetylsuccinate. Background technique [0002] The structural formula of dimethyl acetylsuccinate is as follows: [0003] [0004] Dimethyl acetylsuccinate is a key intermediate in the production of a new type of environmentally friendly dimethyl acetylsuccinate carboxylate ketone food additive -- tartrazine, which is widely used in various foods in Europe and America. Lemon yellow is one of the 6 kinds of food coloring approved by our country. It is stipulated in my country's "Hygienic Standards for the Use of Food Additives" (GB2760-1996) that lemon yellow can be used in fruit juice drinks, prepared wine, candy, cakes, canned food, pickled products, plants, etc. Protein drinks and lactic acid bacteria drinks. [0005] The synthetic method of dimethyl acetylsuccinate reported both at home and abroad is that dimethyl maleate and acetalde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/313
Inventor 任全胜戈建华张国亮张凤宝王淑梅樊新敏
Owner 河北彩客新材料科技股份有限公司
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