Method for preparing dimethyl succinate

A technology of dimethyl succinate and succinic acid, which is applied in the field of preparation of dimethyl succinate, can solve the problems of economic impact on industrial production, easy deactivation, complicated steps, etc., and achieves elimination of the impact of catalyst activity , the effect of increasing the adsorption concentration range and improving the conversion rate of esterification

Active Publication Date: 2017-05-17
SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD +1
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  • Claims
  • Application Information

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Problems solved by technology

[0003] CN1011824627A discloses a method for preparing dimethyl succinate with maleic anhydride and methanol, although the reaction speed is fast and the temperature is low, impurities such as monomethyl fumarate are produced in the reaction process , which affects the product purity, and the whole system has many operating units, which are relatively complicated and the steps are cumbersome, which is not conducive to industrial production
CN102070448A discloses a method for preparing dimethyl succinate. The method uses maleic anhydride to esterify to generate dimethyl maleate, and then obtains dimethyl succinate through hydrogenation. Although the process flow is simple, there is no Pollution, but hydrogenation catalysts use noble metals as active components, which are costly and easy to deactivate, which has a great impact on the economics of industrial production
[0005] The production of dimethyl succinate from biological succinic acid and methanol is a future development trend, but it is difficult to avoid a certain amount of nitrogen in succinic acid products during the production of biological succinic acid, and most of them are ammonia nitrogen Exists in the form of ammonia nitrogen, which will affect the activity and service life of the esterification catalyst. Therefore, eliminating the influence of ammonia nitrogen on the catalyst will be an important problem to be solved

Method used

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  • Method for preparing dimethyl succinate

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Experimental program
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Effect test

Embodiment 1

[0025] Take a certain amount of methanol and succinic acid raw materials for monoesterification reaction in an autoclave, the reaction temperature is 120°C; the reaction pressure is 0.5MPa; the molar ratio of alkyd to acid is 2:1, and the stirring speed is 250rin / min .

[0026] Take 100g of activated carbon, wash 5 times with deionized water at room temperature, 10 minutes each time, filter and react with 25% nitric acid aqueous solution for 3 hours under stirring, the volume ratio of nitric acid aqueous solution to activated carbon is 3:1, The stirring speed is 200rin / min, the reaction temperature is 50°C, and after filtration, it is dried in a vacuum oven for 8 hours at a drying temperature of 90°C, and then roasted at 300°C for 10 hours to obtain activated carbon with 20% ZnSO 4 Aqueous reaction for 4 hours, ZnSO 4 The volume ratio of the aqueous solution to the activated carbon is 4:1, the reaction temperature is 60°C, and after filtration, the reacted activated carbon i...

Embodiment 2

[0029] Take a certain amount of methanol and succinic acid raw materials for monoesterification reaction in an autoclave, the reaction temperature is 120°C; the reaction pressure is 0.5MPa; the molar ratio of alkyd to acid is 2:1, and the stirring speed is 250rin / min .

[0030] Take 100g of activated carbon, wash 5 times with deionized water at room temperature, 10 minutes each time, filter and react with 20% nitric acid aqueous solution for 3 hours while stirring, the volume ratio of nitric acid aqueous solution to activated carbon is 3:1, The stirring speed is 200rin / min, the reaction temperature is 50°C, and after filtration, it is dried in a vacuum oven for 8 hours at a drying temperature of 90°C, and then roasted at 300°C for 10 hours to obtain activated carbon with 15% ZnSO 4 Aqueous reaction for 4 hours, ZnSO 4 The volume ratio of the aqueous solution to the activated carbon is 3:1, the reaction temperature is 60°C, and after filtration, the reacted activated carbon i...

Embodiment 3

[0033] Take a certain amount of methanol and succinic acid raw materials for monoesterification reaction in an autoclave, the reaction temperature is 110°C; the reaction pressure is 0.5MPa; the molar ratio of alkyd to acid is 3:1, and the stirring speed is 250rin / min .

[0034] Take 100g of activated carbon, wash 5 times with deionized water at room temperature, 10 minutes each time, filter and react with 30% nitric acid aqueous solution for 3 hours while stirring, the volume ratio of nitric acid aqueous solution to activated carbon is 4:1, The stirring speed is 200rin / min, the reaction temperature is 50°C, and after filtration, it is dried in a vacuum oven for 8 hours at a drying temperature of 90°C, and then roasted at 300°C for 10 hours to obtain activated carbon with 15% ZnSO 4 Aqueous reaction for 4 hours, ZnSO 4 The volume ratio of aqueous solution to activated carbon is 3:1, and the reaction temperature is 60°C. After filtration, the reacted activated carbon is dried ...

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Abstract

The invention discloses a method for preparing dimethyl succinate. The method comprises the following steps: carrying out an autocatalytic mono-esterification reaction on biological process succinic acid and methanol, and allowing the obtained autocatalytic mono-esterification reaction product to go through a catalytic rectification reaction device provided with an ion exchange resin catalyst and modified active carbon used as an adsorbent and undergo a double esterification reaction in order to generate dimethyl succinate, wherein the ion exchange resin and the modified active carbon are added in a grading manner according to a certain volume ratio, and reaction product flow sequentially goes through a modified active carbon bed A, an ion exchange resin catalyst bed and a modified active carbon bed B. The method has the advantages of effective elimination of influences of ammonia nitrogen in the biological process succinic acid raw material on the dimethyl succinate product and the catalyst, high esterification efficiency, and stable activity and long-time cycle running of the catalyst.

Description

technical field [0001] The invention relates to a method for preparing dimethyl succinate, in particular to a method for preparing dimethyl succinate using biological succinic acid and methanol as raw materials. Background technique [0002] Dimethyl succinate, also known as dimethyl succinate, is generally a colorless crystal or liquid, easily soluble in organic solvents such as ether, methanol, ethanol and acetone, and slightly soluble in water. Widely used in food, spices, daily chemical, pharmaceutical, coating, rubber and plastic industries, used to synthesize light stabilizers, high-grade coatings, fungicides, pharmaceutical intermediates, is an important chemical intermediate, widely used in Raw materials for various chemical products. [0003] CN1011824627A discloses a method for preparing dimethyl succinate with maleic anhydride and methanol, although the reaction speed is fast and the temperature is low, impurities such as monomethyl fumarate are produced in the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/54C07C67/56C07C69/40
CPCC07C67/08C07C67/54C07C67/56C07C69/40Y02P20/10
Inventor 刘野霍稳周李花伊邓玉媛张宝国
Owner SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD
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