Process for preparing dimethyl carbonate catalyst by liquid-phase oxidation carbonylation of methanol

A dimethyl carbonate, liquid-phase oxidation technology, applied in the chemical industry, can solve problems such as easy agglomeration, uneven dispersion, inconvenient transportation and industrial operation, and achieve high activity and selectivity, easy dispersion, and good industrial application foreground effect

Inactive Publication Date: 2015-11-25
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

This patent proposes a new preparation process for the shortcomings of such catalysts, such as easy agglomeration, uneven

Method used

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Examples

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Effect test

example 1

[0009] [Example 1] 10 kg of cuprous chloride and 16 kg of polypyridine were dispersed / dissolved in 10 kg and 16 kg of methanol, respectively, and then the latter solution was added to the preceding suspension. Stir at room temperature for 1 hour at a rotational speed of 50 r / min; transfer the obtained suspension into a vacuum double-cone dryer, and dry at 50° C. for 5 hours at a vacuum degree of -0.09 MPa. The obtained solid catalyst was crushed to 100-200 mesh. In the 100ml batch reactor, add the powder catalyst 0.26g of gained, methyl alcohol 10ml, CO2.7MPa and O 2 0.3MPa, 110°C for 2 hours, methanol conversion rate 30.1%, dimethyl carbonate selectivity 99.9%.

example 2

[0010] [Example 2] The polypyridine is replaced with polyvinylpyridinone, other conditions are the same as in Example 1, the conversion of methanol is 20.1%, and the selectivity of dimethyl carbonate is 99.9%.

example 3

[0011] [Example 3] The solvent is changed from methanol to acetone, and other conditions are the same as in Example 1, the conversion of methanol is 30.3%, and the selectivity of dimethyl carbonate is 99.9%.

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PUM

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Abstract

The invention relates to a process for preparing a dimethyl carbonate catalyst by liquid-phase oxidation carbonylation of methanol. The process comprises the following steps: respectively dispersing or dissolving cuprous halide and one or more of nitrogenous heterocyclic compounds and nitrogen-containing polymers in an organic solvent; adding a solution/suspension into another solution/suspension at a certain temperature and stirring speed, continuously stirring for a certain period to form a coordination complex; transferring the suspension into a vacuum drier, removing the organic solvent at a certain temperature and vacuum degree to obtain a solid powdered catalyst, and grinding the catalyst to 100-200 meshes; and adding a dry powder catalyst, methanol, CO and O2 into a batch reactor, and synthesizing dimethyl carbonate at a temperature of 90-130 DEG C and pressure of 2.0-3.0MPa, wherein the per-pass conversion is more than or equal to 30 percent, and the selectivity of the target product dimethyl carbonate is more than or equal to 99.9 percent. The catalyst is simple in preparation process, cannot be easily caked, and has good activity, selectivity and stability.

Description

technical field [0001] The invention relates to a preparation process of a catalyst for synthesizing dimethyl carbonate by methanol liquid-phase oxidative carbonylation, and belongs to the technical field of chemical industry. Background technique [0002] Since dimethyl carbonate (DMC) was listed as a non-toxic chemical by Europe in 1992, as a "green" chemical product, its synthesis method and application field have been continuously expanded. Dimethyl carbonate contains functional groups such as carbonyl, methyl, methoxy, carboxyl and methoxycarbonyl, and has good reactivity. It is widely used in pesticides, medicines, plastics, dyes, electronic chemicals, food additives and other fields. Dimethyl carbonate can replace phosgene as a carbonylating agent; replace dimethyl sulfate as a methylating agent; it can also be used as a low-toxic solvent for paint solvents and solvents used in the pharmaceutical industry; and it is replacing methyl tert-butyl ether It has very broad...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C69/96C07C68/00
Inventor 邓志勇王公应杨先贵曾毅
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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