Catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate

A technology for catalyzing dimethyl oxalate and dimethyl carbonate, which is applied in the preparation of carbonate/haloformate, catalyst activation/preparation, and preparation of organic compounds, to achieve innovative catalyst synthesis methods, good reactivity, and high selective effect

Pending Publication Date: 2021-07-30
张威
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Since there are no in-depth research and detailed reports on the method of directly generating dimethyl carbonate from the decarbonylation of dimethyl oxalate in the liquid phase system and the preparation method of the catalyst at home and abroad, it is necessary to explore highly active and selective catalysts to realize liquid It is of great significance to prepare carbonate products such as dimethyl carbonate by phase decarbonylation

Method used

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  • Catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate
  • Catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate
  • Catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of Catalyst / Support Complex:

[0044] Dissolve 0.5g of lithium hydroxide and 0.2g of CTAB surfactant in 50mL of deionized water / ethanol (volume ratio 5:1) mixed solvent to form a uniform solution, and then 5g of the specific surface area is 500m 2 / g of nanoporous silica dispersed in the solution, fully impregnated, heated, stirred and dried, and then calcined the obtained solid at 800°C for 3 hours, and a chemical reaction occurred: 2LiOH+SiO 2 = Li 2 SiO 3 +H 2 O, making lithium silicate (Li 2 SiO 3 ) catalyst to obtain a catalyst / support composite.

[0045] Application of catalyst / support complex to catalyze the decarbonylation reaction of dimethyl oxalate:

[0046] Put 5g of the above-prepared catalyst / carrier complex and 500mL of ethylene glycol solvent into a stainless steel autoclave, add 500mL dimethyl oxalate (574g) after preheating to 100°C, seal the autoclave and heat it in an oil bath while stirring To 150°C, argon gas was introduced to ma...

Embodiment 2

[0051] Preparation of Catalyst / Support Complex:

[0052] Dissolve 0.5g of sodium oxalate and 0.2g of SDBS surfactant in 50mL of deionized water / ethanol (volume ratio 5:1) mixed solvent to form a uniform solution; using a specific surface area of ​​800m 2 / g of porous activated carbon was soaked and adsorbed tetraethyl silicate for 1 h, and after taking it out, it was pyrolyzed under argon to obtain activated carbon coated with a silicon dioxide layer. Disperse 5 g of the above-mentioned activated carbon coated with silica layer in sodium oxalate solution, fully impregnate it, heat, stir and dry it, then calcinate the obtained solid at 800°C for 3 hours, and a chemical reaction occurs: Na 2 C 2 o 4 +SiO2 2 →Na 2 SiO 3 +CO+CO 2 , making sodium silicate (Na 2 SiO 3 )catalyst.

[0053] Application of catalyst / support complex to catalyze the decarbonylation reaction of dimethyl oxalate:

[0054] Put 5g of the above-prepared catalyst / carrier complex and 500mL of ethylene g...

Embodiment 3

[0059] Preparation of Catalyst / Support Complex:

[0060] Dissolve 0.8g potassium acetate and 0.2g CTAB surfactant in 50mL deionized water / ethanol (volume ratio 5:1) mixed solvent to form a homogeneous solution. Utilize a specific surface area of ​​500m 2 / g of porous activated carbon was soaked and adsorbed ethyl orthogermanate for 3 hours, and after taking it out, it was pyrolyzed at high temperature under argon to obtain activated carbon coated with a germanium dioxide layer. Disperse 5 g of the above-mentioned activated carbon coated with germanium dioxide layer in potassium acetate solution, fully impregnate it, heat, stir and dry it, and then calcinate the obtained solid at 800 ° C for 3 hours, and a chemical reaction occurs: CH 3 COOK+GeO 2 →K 2 GeO 3 +H 2 O+CO 2 , making potassium germanate (K 2 GeO 3 )catalyst.

[0061] Applied to catalyze the decarbonylation reaction of dimethyl oxalate:

[0062] Put 5g of the catalyst / carrier compound prepared above and 500...

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Abstract

The invention discloses a catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate. According to the invention, alkali / alkaline earth metal third and fourth main group inorganic acid salt catalysts and carriers thereof are prepared and compounded through a volume impregnation method, an in-situ calcination method and the like, and a catalytic system for catalyzing decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate is obtained. The catalytic system has good reaction activity in the decarbonylation reaction of the dimethyl oxalate, the catalytic system is used for realizing the decarbonylation reaction of the dimethyl oxalate in a liquid phase system, and the product dimethyl carbonate can be prepared with high catalytic selectivity and high conversion rate of the dimethyl oxalate.

Description

technical field [0001] The invention relates to a catalytic system for catalyzing the decarbonylation of dimethyl oxalate to directly generate dimethyl carbonate, belonging to the technical field of chemical synthesis. Background technique [0002] With the increasingly prominent substitution of carbonates in gasoline oxygen-containing additives and the sudden increase in the demand for lithium-ion batteries in social development, the demand for dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate in industrial production will definitely increase. increasing day by day. The methods for preparing dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate include traditional phosgene synthesis method, carbon dioxide methanol method, transesterification method, urea methanol method, catalytic oxidation method and the like. It is worth noting that the introduction of nitrite in the preparation of oxalate and carbonate products by carbon monoxide low-pressure g...

Claims

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Application Information

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IPC IPC(8): B01J21/14B01J23/04B01J23/14B01J37/02B01J37/08C07C68/00C07C69/96
CPCB01J37/0213B01J37/0207B01J37/08B01J23/04B01J23/14B01J21/14C07C68/00C07C69/96Y02P20/141
Inventor 张士祥穆仕芳王亚萌张威
Owner 张威
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