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Method for preparing long-chain dicarboxylic dialkyl ester

A technology of chain dicarboxylic acid dialkyl ester and long-chain dicarboxylic acid, which is applied in the field of dialkyl ester preparation, can solve the problems of lowering the reaction rate of esterification, low reaction temperature, and many operation steps, and achieves the improvement of esterification. The effect of reaction rate, shortened operation cycle, and reduced production cost

Inactive Publication Date: 2005-07-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain a satisfactory conversion rate, there are many operating steps, complicated process, high cost and long time, and this resin catalyst can only be used to produce long-chain dicarboxylic acid short-chain dialkyl esters, suitable alkanes base alcohol is C 1 ~C 4 The n-isomeric alcohols are not suitable for the preparation of long-chain dicarboxylic acid dialkyl esters by the reaction of long-chain dicarboxylic acids and high-carbon alcohols, and due to the poor temperature resistance of the catalyst, the esterification reaction temperature can only be maintained at 60-80 °C. Catalyst will lose activity over 100°C
Too low reaction temperature greatly reduces the rate of esterification reaction and cannot remove the water generated by the reaction in time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 60g of refined dodecanedioic acid, 480g of 2-ethylhexanol and 22g of "DNW" cation exchange resin produced by Dandong No. The esterification reaction was carried out at this temperature. During the reaction process, water was continuously evaporated, collected in a receiving bottle, and reacted for 3.5 hours. At this time, no more water was evaporated, and the reaction was terminated. Reaction liquid is distilled under reduced pressure, reclaims unreacted alcohol, then with the NaHCO of 50ml 2N 3 The obtained crude ester was washed with solution (preheated to 60°C), and then washed with hot water at 60°C until neutral. The residual moisture in the crude ester was evaporated under a vacuum degree of 50 kPa to obtain 106.3 g of the product bis(2-ethylhexyl) dodecanedioate, and the esterification recovery rate was 94.6 wt%.

Embodiment 2

[0037] Add 70g of pentadecanedioic acid with bacteria (pentadecanedioic acid content 89.0%), 300g of isotridecanol and 4.2g of Beijing Guanghua Wood Factory "GH-88" powdered activated carbon into 1000ml with reflux condenser In a three-necked flask, heated to 80°C under stirring, decolorized and adsorbed for 1 hour, and the stirring speed was 80r / min. Then filter while hot to obtain the alcohol solution of dicarboxylic acid, add the filtrate into a 500ml three-neck flask with a distillation receiving system, and add 28g of "DNW" cation exchange resin produced by Dandong Chemical No. 3 Factory, and heat the reaction solution to 130°C under stirring , Receive the water evaporated in the reaction process in the receiving bottle, and stop the reaction until no water distills out, and the reaction time is 3.2h. The rest of the steps and conditions were the same as in Example 1, and 136.2 g of diisotridecyl pentadecanedioate was obtained, with an esterification recovery rate of 93.2 w...

Embodiment 3

[0039] Add 60g of refined tridecanedioic acid, 350g of isodecyl alcohol, 2g of 1,2-butanediol and 50g of "DNW" cation exchange resin produced by Dandong Chemical No. The reaction solution was heated to 100°C for esterification reaction, and the reaction was stopped when no water evaporated, and the reaction time was 4.6 hours. Then reclaim unreacted isodecyl alcohol according to the method of Example 1, alkali washing, water washing, dehydration, make tridecanedioic acid diisodecyl-tridecanedioic acid butanediol complex ester 118.2g, esterification recovery Rate 93.8wt%.

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Abstract

The method for preparing long-chain dicarboxylic acid dialkyl ester uses dicarboxylic acid of C8-C18 and excess C6-C18 monobasic alcohol as raw material, adopts proper acidic resin as catalyst, and makes them implement esterification reaction at higher temp., at the same time of esterification the formed water content is evaporated out, the conversion rate of reaction can be raised, and the reaction liquid can be undergone the processes of distillation, etc. and can be purified. Said invention has the advantages of short process, high esterification rate, short operation period, and low energy consumption, etc.

Description

technical field [0001] The invention relates to a method for preparing dialkyl esters from dicarboxylic acids and alkyl alcohols, in particular to a method for preparing long-chain fatty dicarboxylic acid dialkyl esters from long-chain fatty dicarboxylic acids and higher carbon alcohols. Background technique [0002] As an important class of organic chemical intermediates, long-chain dicarboxylic acid dialkyl esters are mainly used as low-temperature plasticizers for plastics, synthetic aviation lubricants, water-based cutting oils, and synthetic spices. Dialkyl dicarboxylates are produced by esterification of dicarboxylic acids with alcohols. The esterification reaction generally needs to be carried out in the presence of an acidic catalyst. The commonly used catalysts are strong inorganic acids such as concentrated sulfuric acid and hydrochloric acid. Although this acidic catalyst has high catalytic efficiency and low price, it is highly corrosive. After the reaction, it n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/34
Inventor 王崇晖宋喜军
Owner CHINA PETROLEUM & CHEM CORP
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