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Process for synthesizing dibutyl carbonate

A technology of dibutyl carbonate and dimethyl carbonate, which is applied in the field of catalytic synthesis of dibutyl carbonate with supported catalysts, can solve the problems of low conversion rate of raw materials, production process, environmental pollution, toxicity, etc., and achieve high conversion rate of raw materials, Ease of separation and mild reaction conditions

Inactive Publication Date: 2005-01-26
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Dialkyl carbonates are used in lithium-ion batteries because of their good electrochemical stability, high flash point and low melting point in the electrochemical field. Among them, dibutyl carbonate has a large Molecular weight, its flash point, oxidation resistance are improved, thereby the electrochemical stability of lithium-ion battery electrolyte and the safety of battery are also improved accordingly (Barker, Jeremy, et al, Carbonaceous electrode and compatible electrolyte [P], U S Patent, 5643 695, 1997; Zhuang Quanchao, Wu Shan, etc., Research on Organic Electrolyte for Lithium-ion Batteries, Vol. VII, No. 4, 2001), there are two main problems in the traditional synthesis method, one is that the method should be a reversible reaction , the conversion rate of raw materials is low, and the other is that the traditionally used carbonylation reagents such as phosgene have certain toxicity, causing great pollution to the production process and the environment. Dimethyl carbonate, a new green chemical, has been Come out, because it is a non-toxic chemical, and because of the superiority of its own structure, it can be used as a carbonylation reagent, or a good methylation reagent, and can replace phosgene, dimethyl sulfate, and methylene chloride Toxic reagents such as dimethyl carbonate have been formed as a new synthetic block (S.Memoli, M.Selva, Dimethylcarbonate foreco-friendly methylation reactions, Chemosphere 43 (2001) 115-121; Yoshio Ono, Dimethyl carbonate for environmentally bengin reactions, Catalysis Today 35 (1997) 15-25)

Method used

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Examples

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Embodiment 1

[0011] The present invention is a process for preparing dibutyl carbonate by using dimethyl carbonate and butanol as raw materials under heterogeneous catalytic reaction conditions. The reaction is carried out in a rotary evaporator, and 0.1mol of industrial grade dimethyl carbonate is used, which is chemically pure. Butanol 0.4mol, supported catalyst KOH / AC2.6g (6% of the raw material quality), wherein the KOH load is 30% of the activated carbon (AC) quality, the oil bath heating temperature is 373K, and the reaction time is 6 hours.

[0012] Since this reaction is a two-step reaction, and both are reversible reactions, the thermodynamic equilibrium constant is very small. In order to break the limitation of thermodynamic equilibrium and improve the conversion rate of raw materials and the selectivity of the target product, 50ml / min of N 2 Pass it into the reaction bottle, take the saturated vapor of methanol out of the reactor, and collect it through a cold trap. After the re...

Embodiment 2

[0014] Industrial grade dimethyl carbonate 0.1mol, chemically pure butanol 0.5mol, supported catalyst KOH / AC2.6g (6% of raw material quality), wherein KOH loading is 10% of activated carbon (AC) quality, oil bath heating The temperature was 363K, the reaction time was 5 hours, other conditions were the same as in Example 1, the conversion rate of dimethyl carbonate was 94.3%, and the selectivity of dibutyl carbonate was 43.26%.

Embodiment 3

[0016] Industrial grade dimethyl carbonate 0.1mol, chemically pure butanol 0.5mol, supported catalyst KOH / AC1.3g (3% of raw material quality), wherein KOH loading is 5% of activated carbon (AC) quality, oil bath heating The temperature was 363K, the reaction time was 5 hours, other conditions were the same as in Example 1, the conversion rate of dimethyl carbonate was 93.88%, and the selectivity of dibutyl carbonate was 38.27%.

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Abstract

The invention discloses a process for synthesizing dibutyl carbonate through the catalysis of load type catalyst, wherein alkali metal hydroxide, alkali metal halides, alkali metal carbonates are loaded onto active aluminium oxide, activated charcoal, or molecular sieve carrier through vacuum dipping method, thus obtaining solid catalyst.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing dibutyl carbonate with a supported catalyst. Background technique [0002] Dialkyl carbonates are used in lithium-ion batteries because of their good electrochemical stability, high flash point and low melting point in the electrochemical field. Among them, dibutyl carbonate has a large Molecular weight, its flash point, oxidation resistance are improved, thereby the electrochemical stability of lithium-ion battery electrolyte and the safety of battery are also improved accordingly (Barker, Jeremy, et al, Carbonaceous electrode and compatible electrolyte [P], U S Patent, 5643 695, 1997; Zhuang Quanchao, Wu Shan, etc., Research on Organic Electrolyte for Lithium-ion Batteries, Vol. VII, No. 4, 2001), there are two main problems in the traditional synthesis method, one is that the method should be a reversible reaction , the conversion rate of raw materials is low, and the other is that th...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96
Inventor 李永昕徐崇福陈兴权
Owner NINGXIA UNIVERSITY
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