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Method for producing 1,6-dimethyl adipate

A technology of dimethyl adipate and production method, which is applied in the field of dimethyl adipate production using solid acid as a catalyst, can solve the problems of large catalyst consumption, complicated process, equipment corrosion, etc., and achieve the elimination of filtration steps, increase conversion rate, and save operating costs

Active Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, the present invention provides a kind of production method of 1,6-dimethyl adipate, and the present invention overcomes the equipment corrosion and pollution problem that traditional technology utilizes sulfuric acid catalyst to bring, and adopts two or more steps One-step catalytic esterification causes complex process and large consumption of catalyst, etc.

Method used

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  • Method for producing 1,6-dimethyl adipate
  • Method for producing 1,6-dimethyl adipate
  • Method for producing 1,6-dimethyl adipate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 pre-esterification experiment

[0024] Mix methanol and adipic acid at an alcohol / acid molar ratio of 3 to 5, heat to an appropriate reaction temperature and reaction pressure (reaction pressure is measured by gauge pressure, and gauge pressure refers to a pressure value higher than atmospheric pressure), under the condition of no catalyst, adipic acid The pre-esterification reaction between the acid and methanol occurred, and the experimental results are shown in Table 1 (the conversion rate of adipic acid is calculated according to the analysis result of the acid value of the product).

[0025] Table 1 Pre-esterification reaction conditions and results

[0026]

Embodiment 2

[0029] Esterification experimental results under different space velocities of embodiment 2

[0030] Utilize the mixed material after the pre-esterification reaction of Example 1 to carry out the continuous esterification experiment, use the DNW-II type resin produced by Dandong Mingzhu Special Resin Co., Ltd. as the catalyst, adopt catalytic rectification reaction, and set 10 blocks in the catalytic rectification tower Trays, the resin catalyst is evenly distributed on each tray. The operating pressure is normal pressure, the temperature at the bottom of the tower is 120°C, and the temperature at the top of the tower is 95°C. The reaction results under different conditions are shown in Table 2.

[0031] Table 2 catalytic rectification esterification reaction conditions and results

[0032]

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Abstract

The invention discloses a method for producing 1,6-dimethyl adipate. The method comprises the following steps of: (1) mixing adipic acid and methanol without adding a catalyst, and performing pre-esterification reaction at the temperature of 80 and 200 DEG C under the gage pressure of between 0.05 and 3 MPa; and (2) conveying materials which are subjected to the pre-esterification reaction to the upper part of a continuous catalytic rectifying tower, and gasifying the dried methanol, conveying to the lower part of the catalytic rectifying tower, allowing the materials which are subjected to the pre-esterification reaction to contact methanol steam in a reverse flow mode in the catalytic rectifying tower and performing esterification reaction further. By the method, the problems of equipment corrosion and pollution which are caused by the utilization of a sulfuric acid catalyst in the conventional process are solved, and the defects of complex processes, large consumption level of the catalyst and the like which are caused by the adoption of two-step or multi-step catalytic esterification are overcome.

Description

technical field [0001] The invention relates to a production method of 1,6-dimethyl adipate, in particular to a production method of dimethyl adipate using solid acid as a catalyst. Background technique [0002] 1,6-Dimethyl adipate is an excellent cold-resistant plasticizer, which can endow products with excellent low-temperature softness, and has certain light-heat stability and water resistance. Dimethyl 1,6-adipate is also an important raw material for organic synthesis and a chemical intermediate, which can be used to produce 1,6-hexanediol through hydrogenation. [0003] At present, the reports on the production method of 1,6-dimethyl adipate include: GB143069 discloses a relatively primitive process method, using concentrated sulfuric acid as a catalyst, and adopting a tank reactor reaction distillation method to remove water. The use of inorganic liquid acid as a catalyst has environmental pollution problems such as corrosion of equipment by the inorganic liquid aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08
Inventor 魏晓霞霍稳周吕清林刘野李花伊
Owner CHINA PETROLEUM & CHEM CORP
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