Process for preparing dimethyl carbonate by reacting methanol, carbon monoxide and oxygen

A technology of dimethyl carbonate and carbon monoxide, which is applied in the preparation of carbon dioxide or inorganic carbonate, chemical instruments and methods, organic chemistry, etc., can solve the problems of reduced corrosion, poor solubility, and difficult separation of products, and achieves a simple catalytic system. , easy separation, and the effect of improving the conversion rate

Inactive Publication Date: 2007-05-16
SHAANXI NORMAL UNIV
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Problems solved by technology

However, due to the poor solubility of CuCl in the reaction system, a high concentration of CuCl must be used in the Enichem process to obtain a sufficient reaction rate; at the same time, CuCl is highly corrosive to the reaction equipment, and glass or enamel lining must be added to the inner wall of the reactor, etc. Anti-corrosion materials; in addition, the process has problems such as catalysts, reactants, and products that are difficult to separate
Chinese patent CN1197792A (1998) uses CuCl as the main catalyst, magnesium chloride, calcium chloride, etc. as auxiliary agents to prepare a composite catalyst modified by alkaline earth metal salts, which improves the solubility of cuprous chloride in the rea

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0014] 4g methyl alcohol and 2gN-butylpyridine tetrafluoroborate ionic liquid and 1mmol CuCl catalyst are joined in the stainless steel high-pressure reactor of 25ml, at room temperature with oxygen and carbon monoxide (O 2 The volume ratio to CO is 1:2) pressurize the reactor to 2.4MPa, and react at 120°C for 2h. After the reaction, it was cooled with an ice-water bath, and the product was analyzed with a gas chromatograph. The conversion rate of methanol was 17.2%, the selectivity of dimethyl carbonate was 97.8%, and the space-time yield of DMC was 4.6gDMC / g·cat·h. The ionic liquid catalytic system was reused 4 times (Example 2-5).

[0015] Table 1 Reuse of CuCl / N-butylpyridine tetrafluoroborate catalytic system for oxidative carbonylation of methanol

[0016] Cycles

Embodiment 6

[0018] No ionic liquid was added to the reaction kettle, and other conditions were the same as in Example 1. The conversion rate of methanol was 9.0%, the selectivity of dimethyl carbonate was 97.3%, and the space-time yield of DMC was 2.3gDMC / g·cat·h.

Embodiment 7

[0020] The N-butylpyridine tetrafluoroborate in Example 1 is replaced with 2g of N-octylpyridine tetrafluoroborate ionic liquid, other conditions are the same as in Example 1, the conversion rate of methanol is 17.2%, and dimethyl carbonate is selected The specificity is 97.8%, and the space-time yield of DMC is 4.6gDMC / g·cat·h.

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PUM

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Abstract

The invention discloses a synthesizing method of dimethyl carbonate through oxidizing and oxonating liquid phase of carbinol in the chemical technological domain, which comprises the following steps: adopting ion liquid as solvent and metal copper salt as catalyst; setting the weight rate of carbinol and ion liquid at 1: 4-10: 1 and the rate of catalyst and carbinol at 1: 100-1: 10; reacting under 80-180 Deg C; setting the initial total pressure of CO and O2 at 0.5-6.0Mpa with the molar rate of CO and O2 at 100: 1-2: 1 for 1-6h; realizing the synthesizing reaction to form dimethyl carbonate with single-course transmission rate at 10-20% and object product selectivity not less than 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing dimethyl carbonate through liquid-phase oxidative carbonylation reaction of methanol, carbon monoxide and oxygen. Background technique [0002] Dimethyl carbonate (DMC) is a high value-added organic chemical raw material, which can replace highly toxic phosgene and dimethyl sulfate as carbonylation reagents, methylation reagents, etc. to manufacture many valuable chemical products. Used in the synthesis of high-performance resins, pharmaceuticals, and pesticide intermediates; it can replace various toxic solvents as solvents for paints and paints; because of its high oxygen content, it can replace methyl tert-butyl ether (MTBE) as a gasoline additive It also has a very broad application prospect. The preparation methods of dimethyl carbonate include phosgene method, methanol oxidative carbonylation method (including liquid phase metho...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/04B01J31/02B01J31/22B01J31/30
CPCY02P20/141
Inventor 董文生周先树刘春玲
Owner SHAANXI NORMAL UNIV
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