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Method for producing dimethyl adipate

A kind of technology of dimethyl adipate, adipic acid

Active Publication Date: 2021-08-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The object of the present invention is to provide the method for producing dimethyl adipate, to overcome the problems such as low conversion rate of acid, high energy consumption, low production capacity and serious pollution in the original process

Method used

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  • Method for producing dimethyl adipate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] This implementation reference figure 1 And illustration.

[0038] The reaction pressure of the primary esterification reactor was 0.5 MpAg; the reaction temperature was 100 ° C.

[0039] The molar ratio of methanol and adipic acid in the primary esterification reactor is 3: 1.

[0040] The esterification reaction rectification tower top pressure is 0.04 MpAg; the tower is mainly adipate dimethyl ester, in order to prevent high temperature coking or decomposition, the tower is 175 ° C.

[0041] The emission reactive distillation tower liquid volume is 0.3h -1 .

[0042] The primary esterification reactor residence time was 2 h, and the conversion of adipic acid was 92% in which the dimethyl dimethyl methalate content was 60% in the formula, 40% ethylene adipate, esterified reaction rectification column Hepa diaphrates have purity = 99.50%, and dimethyl acid value of adipate = 0.5 mgKOH / g can be sold directly as a product, and can also produce 1,6-adipanol products.

Embodiment 2

[0044] This implementation reference figure 1 And illustration.

[0045] The reaction pressure of the primary esterification reactor was 0.6 MpAg; the reaction temperature was 100 ° C.

[0046] The molar ratio of methanol and adipic acid in the primary esterification reactor is 3: 1.

[0047] The esterification reaction rectification tower top pressure is 0.04 MpAg; the tower is mainly adipate dimethyl ester, in order to prevent high temperature coking or decomposition, the tower is 175 ° C.

[0048] The esterification reaction rectification tower liquid volume spatial speed is 0.3h -1 .

[0049] The first-order esterification reactor residence time was 2 h, and the conversion of adipic acid was 92% in which the dimethyl meta of adipate was 62%, 38% ethylene adipate, and the esterification reaction rectification column of adipate. The purity of dimethyl adipate is = 99.52%, the dimethyl acid value of adipate = 0.5 mgkoh / g can be sold directly as a product, and can also produce 1...

Embodiment 3

[0051] This implementation reference figure 1 And illustration.

[0052] The reaction pressure of the primary esterification reactor was 0.8 MpAg; the reaction temperature was 120 ° C.

[0053] The molar ratio of methanol and adipic acid in the primary esterification reactor is 4: 1.

[0054] The esterification reaction rectification tower top pressure is 0.06 MpAg; the tower is mainly adipate dimethyl ester, in order to prevent high temperature coking or decomposition, the tower is 182 ° C.

[0055] The esterification reaction rectification tower liquid volume spatial speed is 0.4h -1 .

[0056] The first-order esterification reactor residence time was 4 h, and the conversion of adipic acid was 94% in which the dimethyl methalate content was 68% in the formula of the ester, 32% of hexahalic acid monolide, esterified reaction distillation column The purity of dimethyl adipate is = 99.65%, the dimethyl acid value of adipate = 0.4 mgkoh / g can be directly sold directly, and can als...

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Abstract

The object of the present invention is to provide the method for producing dimethyl adipate, the method comprises: (1) the adipic acid of fresh methyl alcohol and melting adds primary esterification reactor; (2) primary esterification reactor tube pass The output material enters the upper part of the reaction section of the esterification rectification tower, and the vaporized methanol enters the lower part of the reaction section. The product containing dimethyl adipate is extracted from the bottom of the tower, and the top gas containing dimethyl ether is extracted from the top of the tower without cooling. (3) The non-condensable gas containing dimethyl ether and the liquid phase containing light components are extracted from the top of the methanol recovery tower, and the side line liquid phase is extracted to recover methanol, which is recycled to a The first-grade esterification reactor is used as the heat removal medium, and the heavy components containing water are extracted from the tower; (4) Fresh methanol is used as the reflux liquid of the rectification tower for the esterification reaction, and esters are absorbed from the ascending gas phase at the same time. The method has the advantages of small floor area, high reaction conversion rate, low unit consumption, high product purity and low energy consumption, and can be used for industrial production of dimethyl adipate.

Description

[0001] Invention [0002] The present invention relates to a method of producing dimethyl adipate, a combination of primary esterification and secondary esterification, producing dimethyl adipate. Background technique [0003] Adipate dimethyl ester is a high boiling colorless transparent liquid, soluble in alcohol and ether, but insoluble in water. It is an important difficult volatile solvent, which is widely used in high-grade coatings, synthetic resins, cleaning agents, inks, etc. As an excellent cold-resistant plasticizer, it is possible to give excellent low temperature soft properties, and has a certain photothermal stability and water resistance. There is a wide range of applications in the production of solvents, medical perfume synthesis, papermaking and cellulose resin. Further, dimethyl adipate or synthesis of 1,6-hexanediol is synthesized. [0004] Because concentrated sulfuric acid has dehydrated and oxidative, traditional synthetic adiparlic acid diethylene processes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/44
Inventor 胡松杨卫胜刘银川
Owner CHINA PETROLEUM & CHEM CORP
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