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Method for preparing dimethyl adipate by continuous esterification

A technology of dimethyl adipate and adipic acid, which is applied in the field of continuous esterification to prepare dimethyl adipate, can solve the problems of non-continuous pre-esterification, etc., and achieve the goal of increasing temperature, reducing dosage and improving conversion rate Effect

Active Publication Date: 2016-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for the continuous esterification of adipic acid, which overcomes the problem that the pre-esterification cannot be continued in the process of producing dimethyl adipate through the esterification of adipate

Method used

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  • Method for preparing dimethyl adipate by continuous esterification
  • Method for preparing dimethyl adipate by continuous esterification
  • Method for preparing dimethyl adipate by continuous esterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Pre-esterification experiment

[0027] Mix methanol and adipic acid at an alcohol / acid molar ratio of 3 to 5, and pass through a tubular reactor with a tube length of 5m, an inner diameter of 1cm, and a Statik mixer with 180° twisted blades staggered by 90°. Under the condition of no catalyst, Adipic acid and methanol undergo a pre-esterification reaction, and the experimental results are shown in Table 1 (the conversion rate of adipic acid is calculated according to the results of liquid chromatography analysis).

[0028] Table 1 embodiment 1 pre-esterification reaction result

[0029]

Embodiment 2

[0030] Embodiment 2 pre-esterification test

[0031] Mix methanol and adipic acid at an alcohol / acid molar ratio of 3 to 5, and pass through a tubular reactor with a tube length of 1m, an inner diameter of 1cm, and a Statik mixer with 180° twisted blades staggered by 90°. The reaction time is 2h. Under the condition of no catalyst, adipic acid and methanol undergo a pre-esterification reaction, and the experimental results are shown in Table 2 (the conversion rate of adipic acid is calculated according to the results of liquid chromatography analysis).

[0032] Table 2 embodiment 2 pre-esterification reaction result

[0033] Experiment number

Embodiment 3

[0036] Esterification experimental results under different space velocities of embodiment 3

[0037] The mixed material after the pre-esterification reaction in Example 1 was used to carry out continuous esterification experiments. The DNW-II resin produced by Dandong Mingzhu Special Resin Co., Ltd. was used as the catalyst, and the catalytic rectification reaction was adopted, and 10 blocks were set 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 3.

[0038] Table 3 catalytic rectification esterification reaction conditions and results

[0039]

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Abstract

The invention discloses a method for preparing dimethyl adipate by continuous esterification, comprising the steps of (1) pre-esterifying mixture of adipic acid and methanol in a tubular reactor with an inner component on the catalyst-free condition, wherein the temperature is 90-180 degrees centigrade and the pressure is 0.05-3 MPa; (2), sending the pre-esterified product to upper part of a continuous catalytic rectifying tower; enabling the dried methanol to enter the lower part of the catalytic rectifying tower after being vaporized; enabling the pre-esterified material to contact the methanol steam in the catalytic rectifying tower in a counter-current manner; and further performing esterifying. The method overcomes the problems that the traditional process has device corrosion and pollution problem caused by the sulphuric acid catalyst, and has no continuous pre-esterification and large catalyst consumption.

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 Patents(China)
IPC IPC(8): C07C69/44C07C67/08
Inventor 魏晓霞霍稳周
Owner CHINA PETROLEUM & CHEM CORP
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