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A kind of catalyst for synthesizing dimethyl carbonate and its preparation method and application

A technology of dimethyl carbonate and catalyst, applied in the field of synthesizing dimethyl carbonate catalyst and preparation thereof, can solve the problems of difficult separation of homogeneous catalyst, low equilibrium conversion rate, etc., and achieves easy recovery and separation, simple preparation method, and improved product quality. quality effect

Active Publication Date: 2017-08-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the disadvantages of low equilibrium conversion rate and difficult separation of homogeneous catalysts in the existing technology of urea and methanol to dimethyl carbonate, the present invention provides a catalyst for urea and methanol to dimethyl carbonate and its preparation method and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] (1) Take 38g of zinc nitrate, dissolve it in 42ml of distilled water, and stir evenly until the zinc nitrate is completely dissolved;

[0024] (2) Add n-butanol and ethyl orthosilicate to the solution in step (1), the molar ratio of n-butanol to ethyl orthosilicate added is 2.1; the molar ratio of water in the solution to ethyl orthosilicate added to 10, continue to stir evenly, drop nitric acid into the solution, and adjust the pH value of the solution to 3;

[0025] (3) Stir the solution in step (2) at 90°C for 3 hours until the solution turns into a gel, and then age at room temperature for 12 hours.

[0026] (4) The gel obtained in step (3) was dried at 100° C. for 10 h, and ground to obtain the final supported catalyst. The amount of active metal zinc is 15%, and the rest is SiO 2 .

[0027] Catalyst evaluation was carried out in an autoclave reactor, using urea and methanol as raw materials, including 15g of urea, 136g of methanol, 27g of catalyst mass, the rea...

example 2

[0029] (1) Take 30g of cerous nitrate, dissolve it in 45ml of distilled water, and stir evenly until the cerous nitrate is completely dissolved;

[0030] (2) Add n-butanol and tetraethyl orthosilicate to the solution in step (1), the molar ratio of n-butanol to tetraethyl orthosilicate is 3; the molar ratio of water in the solution to the added tetraethyl orthosilicate to 14, continue to stir evenly, drop nitric acid into the solution, and adjust the pH value of the solution to 4;

[0031] (3) The solution in step (2) was stirred at 80°C for 2 hours to convert the solution into a gel, and then aged at room temperature for 24 hours.

[0032] (4) The gel obtained in step (3) was dried at 100° C. for 12 hours, and ground to obtain the final supported catalyst. The amount of active metal cerium is 11%, and the rest is SiO 2 .

[0033] Catalyst evaluation was carried out in an autoclave reactor, using urea and methanol as raw materials, including 18g of urea, 116g of methanol, 1...

example 3

[0035] (1) Take 32g of cerous nitrate, dissolve it in 40ml of distilled water, and stir evenly until the cerous nitrate is completely dissolved;

[0036] (2) Add n-butanol and tetraethyl orthosilicate to the solution in step (1), the molar ratio of n-butanol to tetraethyl orthosilicate is 1.0; the molar ratio of water in the solution to the added tetraethyl orthosilicate to 9, continue to stir evenly, drop nitric acid into the solution, and adjust the pH value of the solution to 4;

[0037] (3) The solution in step (2) was stirred at 80°C for 2.5h to convert the solution into a gel, and then aged at room temperature for 16h.

[0038] (4) The gel obtained in step (3) was dried at 70° C. for 14 hours, and ground to obtain the final supported catalyst. The amount of active metal cerium is 8%, and the rest is SiO 2 .

[0039] Catalyst evaluation was carried out in an autoclave reactor, using urea and methanol as raw materials, including 15g of urea, 95g of methanol, 17g of cata...

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Abstract

The invention discloses a preparation method of a supported catalyst for preparing dimethyl carbonate from urea and methanol, which comprises the following contents: (1) adding metal salts or metal oxides to distilled water and stirring evenly; (2) adding 1) Add alcohol solvent and silicon-containing precursor to the solution, stir the solution evenly, and adjust the pH value of the solution to 2~5; (3) Stir the solution in step (2) at constant temperature until it turns into a gel, and age at room temperature; (4 ) drying the gel obtained in step (3) to constant weight, and grinding to obtain the final loaded urea and methanol-to-dimethyl carbonate catalyst. The catalyst prepared by the method solves the problems of low equilibrium conversion rate and difficult separation of homogeneous catalysts in the existing urea and methanol production technology of dimethyl carbonate, and the catalyst has high activity and stability.

Description

technical field [0001] The invention relates to a catalyst for synthesizing dimethyl carbonate and its preparation method and application, in particular to a catalyst for preparing dimethyl carbonate from urea and methanol, its preparation method and application. Background technique [0002] Dimethyl carbonate (DMC) is an environmentally friendly organic chemical raw material that meets the requirements of modern "clean technology", and is one of the green chemical products unanimously recognized by the international community. It can not only replace phosgene, dimethyl sulfate, methyl chloride and methyl chloroformate as reagents for carbonylation, methylation, esterification and transesterification, but also be a good green solvent and gasoline additive. [0003] Catalytic synthesis of dimethyl carbonate (DMC) by alcoholysis of methanol and urea is a novel process route to replace phosgene to produce DMC. The urea alcoholysis method uses urea and methanol, which are wide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/06B01J23/10C07C69/96C07C68/00
Inventor 孙潇磊尹泽群宋喜军刘全杰张志智张喜文
Owner CHINA PETROLEUM & CHEM CORP