Catalyst used for catalytic synthesizing dimethyl carbonate directly from methanol and carbon dioxide and preparation and using method thereof

A technology of dimethyl carbonate and carbon dioxide, which is applied in the field of catalysts for the synthesis of dimethyl carbonate, can solve the problems of low conversion rate target product selectivity, difficulty in realizing industrial production, and difficult reaction process, so as to achieve easy separation and easy operation , highly selective effect

Inactive Publication Date: 2008-03-19
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalytic systems used, including alkaline earth metal alkoxylates, bases, acetates, organometallic tin, titanium alkoxylates, supported metals, zirconium dioxide, ceria, organotin and ionic liquids class, etc., but the main problem is that the conversion rate of the reactant and the selectivity of the target product are low, and the reaction process is difficult to control, so it is difficult to realize industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Accurately weigh 10g of natural graphite, slowly add it into 230ml of concentrated sulfuric acid (98%) cooled in an ice-water bath to below 4°C under stirring, then slowly add 5g of sodium nitrate and 28g of potassium permanganate, and stir for 10 minutes. Remove the ice bath, transfer the reaction system to a hot water bath at 36°C and stir for 30 minutes, then stir and react at 95°C in an oil bath for 1 hour, and the product is fully washed with 5% hydrochloric acid and deionized water, ℃ in a vacuum drying oven for 24 hours to obtain a graphite oxide carrier;

[0025] Accurately weigh 0.822gCu(NO 3 ) 2 .3H 2 O and 0.494gNi(NO 3 ) 2 .6H 2 Dissolve O in 30ml of absolute ethanol, impregnate 2g of graphite oxide carrier into the above metal salt solution, stir at room temperature for 2 hours, ultrasonically disperse for 1 hour, stand at room temperature for 12 hours, dry at 40°C for 2 hours, and dry at 60°C 4 hours, then dried at 90°C for 12 hours, and then cooled ...

Embodiment 2

[0028] Carrier preparation method is the same as embodiment 1, and 2g graphite oxide carrier is impregnated to 0.4116gCu(NO 3 ) 2 .3H 2 O and 0.2476gNi(NO 3 ) 2 .6H 2 In the metal salt solution of O, all the other preparation and test conditions are the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0030] Catalyst preparation conditions are the same as in Example 1, and the catalytic reaction conditions are; temperature 120°C, pressure 1.2MPa, raw material molar ratio (methanol / carbon dioxide=2 / 1), and all the other test conditions are the same as in Example 1. The results are shown in Table 1.

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PUM

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Abstract

The invention discloses a direct catalytic synthesis catalyst to prepare dimethyl carbonate from methanol and carbon dioxide and the preparation and application methods of the catalyst. The catalyst of the invention consists of transitional metal soluble salt, promoter and carrier, with the weight ration from 0.01to 0.5: 0.01to 0.1:1. The preparation method is that: (1) the carrier is impregnated into the transition metal soluble salt solution; (2) the promoter is added into the solution, which is stirred in room temperature, ultrasonically dispersed and stored stationarily in room temperature; (3) the solution is dried, sintered, reduced and activated to produce catalyst. The application method is that: the catalyst is put in high pressure reactor or micro reaction device with the temperature of the catalyst bed controlled between 90 degrees centigrade to 140 degrees centigrade and the reaction pressure between 0.6 to 3.0MPa. The catalyst is applicable in direct catalytic synthesis to prepare dimethyl carbonate from methanol and carbon dioxide. The raw material sources are rich, the cost is low, the preparation method is simple and the operation is easy. The catalyst is easily separated from the products, the reaction conditions are mild and the catalyst can be used repeatedly. The catalyst has high activity and selectivity.

Description

technical field [0001] The invention relates to a catalyst for synthesizing dimethyl carbonate, a preparation method and a use method. Background technique [0002] Dimethyl carbonate (DMC) is an important organic synthesis intermediate, known as the "new template" of organic synthesis, which can replace highly toxic or carcinogenic phosgene, methyl chloroformate, dimethyl sulfate and formazan Substances such as base chloride are used as carbonylation, methylation and methoxylation reagents, and can be used as environmentally friendly intermediates and starting materials for organic synthesis. In recent years, DMC has been widely used in the preparation of high-performance resins, solvents, dye intermediates, pharmaceutical additives, food preservatives, fuel additives and other fields, and has attracted increasing attention. At present, there are a large number of patents published on the production and application of DMC at home and abroad, and there has been a certain sc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/72C07C69/96C07C68/04
CPCY02P20/141
Inventor 孟跃中卞军肖敏杜风光王拴紧王晓锦徐艳
Owner SUN YAT SEN UNIV
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