Process for preparing dibasic acid ester

A technology of dibasic acid esters and dibasic carboxylic acids, which is applied in the field of preparing dibasic acid esters, and can solve problems such as unfavorable continuous industrial production

Active Publication Date: 2008-09-17
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Also have is the batch operation that is carried out under stirring condition, and adopts batch reaction to be unfavorable for the continuous industrial production of large-scale

Method used

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  • Process for preparing dibasic acid ester

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Experimental program
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Effect test

Embodiment 1

[0022] (1). In the pre-esterification kettle 1, a solid acid catalyst is first added from the feed port, and the dicarboxylic acid or dicarboxylic acid mixture is added into the pre-esterification kettle 1 from the feed port of the pre-esterification kettle; Alcohol is fed into the pre-esterification kettle 1 from the low-carbon alcohol intermediate storage tank with an intermittent feed pump. In normal operation, the solid acid catalyst is stored in the kettle for repeated use. Based on the quality of dicarboxylic acid or dicarboxylic acid mixture, the amount of solid acid catalyst added is 1% to 10% of dicarboxylic acid or dicarboxylic acid mixture, and the preferred amount is 3% to 7%. ; The alkyd-acid molar ratio is 1-10, and the preferred alkyd-acid molar ratio is 2-5.

[0023] (2). Heating the pre-esterification tank, the low-carbon alcohol vapor discharged from the pre-esterification tank during the reaction is condensed and then returned to the pre-esterification reac...

Embodiment 2

[0031] Add solid acid catalyst, adipic acid and methanol in the esterification kettle, heat and stir at normal pressure, and carry out pre-esterification reaction. The amount of catalyst added is based on the quality of adipic acid. The specific results are as follows:

[0032] Table 1 Adipic acid and methanol pre-esterification experimental results

[0033] Catalyst added

Embodiment 3

[0035] Add solid acid catalyst, glutaric acid and methanol in the esterification kettle, under normal pressure, heat and stir, and carry out pre-esterification reaction. The amount of catalyst added is based on the quality of glutaric acid. The specific results are as follows:

[0036] Table 2 Glutaric acid and methanol pre-esterification experimental results

[0037] Catalyst added

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Abstract

The invention relates to a method of preparing dibasic acid esters. Solid acid catalyst, dualistic carboxylic acid or dualistic carboxylic acid mixture, and low-carbon alcohol are added in a pre-esterification kettle; the addition amount of the solid acid catalyst is 1 to 10 percent of the quality of the dualistic carboxylic acid or the dualistic carboxylic acid mixture; the molar ratio of the alcohol and the dualistic carboxylic acid or the dualistic carboxylic acid mixture is 1 to 10:1; the reaction is performed under the normal atmosphere, wherein, the temperature ranges from 50 to 100 DEG C; the supernatant fluid of reaction products is delivered into the upper part of an esterification reactor; after the low-carbon alcohol is turned into vapour by passing through a carburetor, the low-carbon alcohol vapour enters into the lower part of the esterification reactor; the supernatant fluid and the low-carbon alcohol vapour effect the reflux reaction at a catalyst section of a continuous esterification reactor; reaction products are expelled from the bottom of the esterification reactor, and unreacted low-carbon alcohol and generated water are steamed from the top of the reactor; esterification reaction occurs under the normal atmosphere, the temperature ranges from 70 to 150 DEG C, the liquid airspeed is 0.1 to 0.7Kg / Kg*h, the airspeed of the low-carbon alcohol is 0.1 to 1.0Kg / Kg*h, and the percent conversion can reach more than 99 percent.

Description

Technical field: [0001] The invention relates to a method for preparing dibasic acid esters. Background technique: [0002] Dibasic esters are excellent cold-resistant plasticizers, which can endow products with excellent low-temperature softness, and have certain light and heat stability and water resistance. [0003] The prior art uses sulfuric acid or other inorganic liquid acids as catalysts to produce carboxylic acid esters, or reacts under certain pressure and higher temperature. The use of inorganic liquid acid as a catalyst has environmental pollution problems such as corrosion of equipment by inorganic liquid acid and treatment of three wastes of reaction products. For example, the disclosed process method of British Patent (GB143069) is: use concentrated sulfuric acid as catalyst, adopt tank reactor reaction, and the method for distilling removes water. [0004] Also have is the batch operation that carries out under stirring condition, and adopts batch reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/34
Inventor 程光剑石鸣彦史君张元礼李凤鸣李民黄集钺姜明吴飞娄阳于春江
Owner PETROCHINA CO LTD
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