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Method for preparing diester succinate by esterifying diammonium succinate

A technology of diammonium succinate and succinate diester, which is applied in the field of preparing dimethyl succinate, can solve the problems of difficult acquisition of main raw materials, long product separation process, unfavorable industrial production, etc., and achieve good product quality , less corrosion, and the effect of inhibiting by-products

Active Publication Date: 2012-10-17
TANGSHAN XUYANG CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product separation process of this method is long, consumes a lot of energy, and the main raw materials are not easy to obtain, which is not conducive to large-scale industrial production.

Method used

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  • Method for preparing diester succinate by esterifying diammonium succinate
  • Method for preparing diester succinate by esterifying diammonium succinate
  • Method for preparing diester succinate by esterifying diammonium succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 7.6g diammonium succinate is added to 11.4% water, and the solution that obtains 19g diammonium succinate mass concentration is 40%, this solution and 20ml methyl alcohol co-flow join in the reactor, add catalyzer simultaneously (SiO 2 -Al 2 o 3 ) 0.6g, feed nitrogen into the reactor to increase the pressure inside the reactor to 0.2Mpa. The reaction temperature is 120° C., and the reaction time is 10 h.

[0030] The number of plates in the succinic acid diester azeotropic distillation tower is 15, 16g of ethyl acetate is added as an entrainer, the reflux ratio is 1, the temperature at the top of the tower is 62-65°C, and the temperature at the bottom of the tower is 90-100°C . The mass spectrogram of the obtained succinic acid diester is as follows figure 1 As shown, the NMR spectrum is shown as figure 2 shown.

[0031] See Table 1 for the experimental results.

Embodiment 2

[0033] 7.6g diammonium succinate is added to 7.6 g of water to obtain 15.2g diammonium succinate mass concentration is a solution of 50%, the solution and 20ml methyl alcohol are added to the reaction kettle concurrently, while adding catalyst (SiO 2 -Al 2 o 3 ) 0.6g, feed nitrogen into the reactor to increase the pressure inside the reactor to 0.2Mpa. The reaction temperature is 150° C., and the reaction time is 10 h.

[0034] The number of plates in the succinic acid diester azeotropic distillation column is 15, 16g of ethyl acetate is added as an entrainer, the reflux ratio is 1, the temperature at the top of the tower is 60-65°C, and the temperature at the bottom of the tower is 90-100°C . The mass spectrogram of the obtained succinic acid diester is as follows figure 1 As shown, the NMR spectrum is shown as figure 2 shown.

[0035] See Table 1 for the experimental results.

Embodiment 3

[0037] 7.6g diammonium succinate is added to 5.07 g of water to obtain 12.67g diammonium succinate mass concentration is a solution of 60%, the solution and 20ml methyl alcohol are added to the reaction kettle in parallel, while adding catalyst (SiO 2 -Al 2 o 3 ) 0.6g, feed nitrogen into the reactor to increase the pressure inside the reactor to 0.2Mpa. The reaction temperature is 150° C., and the reaction time is 10 h.

[0038] The number of plates of the succinate azeotropic distillation column is 15, 16g of ethyl acetate is added as an entrainer, the reflux ratio is 1, the temperature at the top of the tower is 60-65°C, and the temperature at the bottom of the tower is 90-100°C. The mass spectrogram of the obtained succinic acid diester is as follows figure 1 As shown, the NMR spectrum is shown as figure 2 shown.

[0039] See Table 1 for the experimental results.

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Abstract

The invention discloses a method for preparing diester succinate by esterifying diammonium succinate, belonging to the field of chemical technology, and particularly discloses a method for preparing the diester succinate product with the purity of more than 99.8% by taking diammonium succinate as a raw material, contacting the raw material with an esterifying agent in a reactor filled with solid acid catalyst to generate dimethyl succinate crude product and finally refining. The method is simple, mild in technological conditions, reasonable in process flow, less in side reaction, high in product purity and good in quality.

Description

technical field [0001] The invention relates to a method for preparing succinate diester through esterification of diammonium succinate, in particular to a method for preparing dimethyl succinate with diammonium succinate and methanol as raw materials. Background technique [0002] Dimethyl succinate (also known as dimethyl succinate, CAS: 106-65-0) is an important synthetic spice and food additive, and is also an intermediate in organic synthesis and pharmaceutical synthesis. It is widely used in food, spices, Daily chemical, pharmaceutical, paint, rubber, plastic and other industries. [0003] Industrially, dimethyl succinate is obtained by esterification reaction with succinic acid and methanol as raw materials under the catalysis of concentrated sulfuric acid catalyst. The esterification reaction using concentrated sulfuric acid as a catalyst has many side reactions, low product yield, strong corrosiveness of sulfuric acid, complex post-treatment, serious pollution, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/40C07C67/08
Inventor 张英伟刘康张新志孙长江
Owner TANGSHAN XUYANG CHEM IND CO LTD
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