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Preparation method of capacitor-grade 2,7-dibutyl octanedioic acid

A technology of dialkoxycarbonyl suberic acid diester and n-butyl malonate diester, which is applied in the synthesis of 2,7-dibutyl suberic acid by phase transfer catalysis, capacitor grade 2,7-di The production field of butyl suberic acid can solve the problems of harsh reaction conditions, troublesome post-processing, complicated process, etc., and achieve the effect of short reaction time, fast reaction speed and simple process

Inactive Publication Date: 2018-05-18
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to solve the technical problems such as harsh reaction conditions, complex process, high cost and troublesome post-processing in the prior art, and improve a high-efficiency, low-cost production of capacitor grade 2,7-dibutylsuberic acid new method

Method used

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  • Preparation method of capacitor-grade 2,7-dibutyl octanedioic acid
  • Preparation method of capacitor-grade 2,7-dibutyl octanedioic acid
  • Preparation method of capacitor-grade 2,7-dibutyl octanedioic acid

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Experimental program
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Effect test

Embodiment 1

[0033] Step (1): 160.2Kg (1Kmol) diethyl malonate, 101.8Kg (1.1Kmol) chlorobutane, 165.9Kg (1.2Kmol) potassium carbonate and 16.1Kg (0.05Kmol) tetrabutylammonium bromide Add it into the reaction kettle, heat to reflux under stirring, react for 2h, after the reaction is completed, cool and filter, and the filtrate is distilled to remove unreacted diethyl malonate and chlorobutane to obtain n-butyl propane The mixed solution of diethyl diethyl malonate and phase transfer agent was used for subsequent use, and the yield of diethyl n-butylmalonate was 78.6%.

[0034]Step (2): 170Kg (0.786Kmol) n-butyl diethyl malonate obtained above, 16.1Kg (0.05Kmol) tetrabutylammonium bromide, 67.9Kg (0.31Kmol) 1,4-dibromobutyl Alkanes, 150Kg (0.9Kmol) of potassium carbonate were added to the reactor, heated to reflux under stirring, reacted for 4h, after the reaction was completed, cooled and filtered, the filtrate was rectified to obtain 2,7-dibutyl-2,7-di Diethyl ethoxycarbonyl suberate, the...

Embodiment 2

[0038] Step (1): 132.2Kg (1Kmol) dimethyl malonate, 103.7Kg (1.12Kmol) chlorobutane, 358.4Kg (1.1Kmol) cesium carbonate and 14.6Kg (0.04Kmol) cetyl trimethyl Ammonium bromide was added to the reaction kettle, heated to reflux under stirring, and reacted for 2.5h. After the reaction was completed, it was cooled and filtered, and the filtrate was distilled to remove unreacted dimethyl malonate and chlorobutane to obtain The mixed solution of dimethyl n-butylmalonate and phase transfer agent is ready for use, and the yield of dimethyl n-butylmalonate is 80.5%.

[0039] Step (2): 151.5Kg (0.805Kmol) dimethyl n-butylmalonate, 14.6Kg (0.04Kmol) hexadecyltrimethylammonium bromide, 78.2Kg (0.36Kmol) 1 obtained above, Add 4-dibromobutane and 275.4Kg (0.85Kmol) cesium carbonate into the reactor, heat to reflux under stirring, react for 3.5h, after the reaction is completed, cool and filter, and the filtrate is rectified to obtain 2,7-dibutyl Dimethyl-2,7-dimethoxycarbonyl suberate with...

Embodiment 3

[0043] Step (1): 188.2Kg (1Kmol) dipropyl malonate, 111.1Kg (1.2Kmol) chlorobutane, 193.5Kg (1.4Kmol) potassium carbonate and 32Kg (0.1Kmol) hexadecyl trimethyl Ammonium chloride was added to the reaction kettle, heated to reflux under stirring, and reacted for 1 hour. After the reaction was completed, it was cooled and filtered, and the filtrate was distilled to remove unreacted dipropyl malonate and chlorobutane to obtain n-butyl The mixed solution of dipropyl butyl malonate and phase transfer agent is standby, and the yield of dipropyl n-butyl malonate is 72.5%.

[0044] Step (2): 177.1Kg (0.725Kmol) n-butyl malonate dipropyl ester obtained above, 32Kg (0.1Kmol) cetyltrimethylammonium chloride, 78.2Kg (0.36Kmol) 1,4 - Dibromobutane and 120.2Kg (0.87Kmol) potassium carbonate were added to the reactor, heated to reflux under stirring, and reacted for 2h. After the reaction was completed, cooled and filtered, the filtrate was rectified to obtain 2,7-dibutyl- Dipropyl 2,7-dipr...

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Abstract

The invention relates to a production method of capacitor-grade 2,7-dibutyl octanedioic acid. The method comprises the steps as follows: diester malonate and chlorobutane as raw materials are subjected to alkylation reaction under the action of alkali with a phase transfer catalysis method, and diester butylmalonate is obtained; then, diester butylmalonate and 1,4-dichlorobutane are subjected to alkylation reaction under the action of alkali, 2,7-dibutyl-2,7-dialkoxycarbonyl octanedioic acid diester is obtained and subjected to saponification, acidolysis and decarboxylation reactions, and 2,7-dibutyl octanedioic acid is obtained. According to the method, the speed of the phase transfer catalysis alkylation reaction is high, and reaction time is short; reaction conditions are mild, few byproducts are produced, and no 'three wastes' is emitted. The method is simple in process, high in product yield and low in cost, and industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a production method of capacitance-grade 2,7-dibutyl suberic acid, in particular to a method for synthesizing 2,7-dibutyl suberic acid by phase transfer catalysis method. Background technique [0002] With the continuous development and expansion of the electronics industry and new electronic products, electrolytic capacitors have also been unprecedentedly developed and widely used, such as communication equipment, computers, automotive electronics, household appliances and other related electronic products. Electrolytic capacitors are widely used, and their demand The volume is huge and increasing year by year. The working environment of these capacitors often requires fast charging and discharging, so the working electrolyte needs to have the characteristics of high conductivity, high flash voltage, high oxidation efficiency, low saturated vapor pressure and stable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/38C07C55/02H01G9/022
CPCC07C51/02C07C51/38C07C51/412H01G9/022C07C55/02C07C55/24
Inventor 罗辉张永闯范维玉南国枝
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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