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Method for preparing didodecyl carbonate by taking oxometallate ion liquid as catalyst

An ionic liquid, dimethyl carbonate technology, applied in the preparation of organic carbonate, organic chemistry and other directions, can solve the problems of complex preparation process of solid base catalyst, poor catalyst reaction activity, harsh reaction conditions, etc., to achieve mild reaction conditions, synthetic Simple method and good stability

Active Publication Date: 2016-03-30
JIANGXI NORMAL UNIVERSITY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, in the above literatures, the preparation process of solid base catalysts is complicated, long-term impregnation and high-temperature roasting are required, and the reaction conditions are harsh.
[0004] The catalyst has many disadvantages such as poor reactivity, low product yield, and easy deactivation of the catalyst.

Method used

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  • Method for preparing didodecyl carbonate by taking oxometallate ion liquid as catalyst
  • Method for preparing didodecyl carbonate by taking oxometallate ion liquid as catalyst
  • Method for preparing didodecyl carbonate by taking oxometallate ion liquid as catalyst

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Experimental program
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Effect test

Embodiment 1

[0019] In the reaction kettle, 18g (0.2mol) of dimethyl carbonate, 111.75g ​​(0.6mol) of lauryl alcohol and 0.649g (accounting for 0.5% of the total mass of raw materials) of 1-ethyl-3-methylimidazolium tungstate ionic liquid were successively added. wt%), stirred and heated to a reaction temperature of 90° C., reacted at a constant temperature for 3 hours, and analyzed by gas chromatography. The conversion rate of dimethyl carbonate was 95%, and the yield of dilauryl carbonate was 90%.

Embodiment 2

[0021] In the reactor, add dimethyl carbonate 18g (0.2mol), lauryl alcohol 74.5g (0.4mol) and 1-propyl-3-methylimidazolium tungstate ionic liquid 1.85g (accounting for 2wt of the total mass of raw materials) successively. %), stirred and heated to a reaction temperature of 100° C., reacted at a constant temperature for 3 hours, and analyzed by gas chromatography. The conversion rate of dimethyl carbonate was 96%, and the yield of dilauryl carbonate was 92%.

Embodiment 3

[0023] In the reactor, add dimethyl carbonate 18g (0.2mol), lauryl alcohol 74.5g (0.4mol) and 1-butyl-3-methylimidazolium tungstate ionic liquid 0.925g (accounting for 1wt of the total mass of raw materials) successively. %), stirred and heated to a reaction temperature of 110° C., reacted at a constant temperature for 2 hours, and analyzed by gas chromatography. The conversion rate of dimethyl carbonate was 99%, and the yield of dilauryl carbonate was 97%.

[0024] After the reaction, reclaim the 1-butyl-3-methylimidazolium tungstate ionic liquid catalyst, and carry out 10 cycle experiments successively according to the above reaction conditions, and the conversion rate of dimethyl carbonate detected by gas chromatography remains at 98% all the time ~99%, the yield of dilauryl carbonate is maintained at 96% ~ 97%.

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Abstract

The invention discloses a method for preparing didodecyl carbonate by taking an oxometallate ion liquid as a catalyst. The method comprises: adding dimethyl carbonate, laurinol and the oxometallate ion liquid catalyst into a reaction kettle in sequence; stirring and heating to 80-110 DEG C; performing a constant-temperature reaction for 1-3 hours and cooling; and performing water-washing, phase-splitting and reduced pressure distillation separation to obtain didodecyl carbonate. According to the method, the oxometallate ion liquid catalyst is high in catalytic activity, the reaction condition is mild, the highest conversion rate of dimethyl carbonate reaches 99%, and the yield of the didodecyl carbonate reaches 97%; and in addition, the oxometallate ion liquid catalyst is simple to synthesize and high in stability, can be reused after water-washing and drying treatment, and still can keep relatively high catalytic activity after being used for multiple times, so that the problems that an existing solid base catalyst is complicated in preparation and liable to lose activity are solved.

Description

technical field [0001] The invention relates to a method for preparing dilauryl carbonate, in particular to a method for preparing dilauryl carbonate by using an oxometalate ionic liquid as a catalyst. Background technique [0002] Dilauryl carbonate is an important organic chemical intermediate, which has good lubricity, wear resistance and corrosion resistance, and is widely used in lubricating oil base oil, textile, polymer and other industries. The traditional method of synthesizing dilauryl carbonate is mainly the phosgene method. Because the raw material phosgene is a highly toxic substance, and the by-product hydrogen chloride is very corrosive to equipment, as people's awareness of environmental protection gradually strengthens, many countries have begun to ban it. Use the phosgene method. In recent years, non-phosgene synthesis of dilauryl carbonate such as oxidative carbonylation, urea alcoholysis and transesterification has developed rapidly and has become a rese...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96
CPCC07C68/06C07C69/96
Inventor 陶端健周言胡文静陈凤凤黄伟
Owner JIANGXI NORMAL UNIVERSITY
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