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Method for indirectly synthesizing dimethyl carbonate by CO gas phase oxidative coupling and decarbonylation

A technology of dimethyl carbonate and oxidative coupling, applied in the preparation of carbonate/haloformate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of propylene oxide dependence and disadvantageous synthesis of dimethyl carbonate Promotion and development, shortage of crude oil resources, etc., to achieve the effects of mild reaction conditions, low prices, and reduced production costs

Inactive Publication Date: 2011-06-01
江苏丹化煤制化学品工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the propylene oxide required for this process depends on petroleum resources and is greatly affected by fluctuations in petroleum prices
my country's energy status is rich in coal, lack of gas, less oil, relatively short of crude oil resources, and the raw material propylene oxide used in the transesterification method comes from non-renewable petroleum resources, which is objectively unfavorable for the synthesis of dimethyl carbonate by transesterification. my country's promotion and development

Method used

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  • Method for indirectly synthesizing dimethyl carbonate by CO gas phase oxidative coupling and decarbonylation
  • Method for indirectly synthesizing dimethyl carbonate by CO gas phase oxidative coupling and decarbonylation
  • Method for indirectly synthesizing dimethyl carbonate by CO gas phase oxidative coupling and decarbonylation

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Experimental program
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Effect test

Embodiment 1

[0031] Preparation of Pd-based catalyst: mix palladium chloride, hydrochloric acid and deionized water to make an impregnation solution, the mass percentage of Pd in ​​the impregnation solution is 1.5%, the volume ratio of the impregnation solution to the carrier is 1.5:1, take 90g of α -A1 2 o 3Dissolve in the above impregnating solution, and heat to 70°C, stir at this temperature for 2h, then impregnate at room temperature for 14h; then filter, and wash the obtained catalyst with deionized water 10 times, each time the amount of deionized water is 500ml, Then they were dried at 60°C for 6h, at 100°C for 15h, and fired at 450°C for 10h. Finally, soak the calcined catalyst in hydrazine hydrate solution at room temperature for 6 hours for reduction, and then wash it with methanol with a concentration of 100% by mass to obtain the final catalyst, which is dried in the air for use.

[0032] Oxidative coupling reaction: Take 100ml of Pd-based catalyst and place it in the constan...

Embodiment 2

[0035] The preparation method of Pd series catalyst is the same as embodiment 1.

[0036] Oxidative coupling reaction: Take 100ml of Pd-based catalyst and place it in the constant temperature zone of the fixed-bed reactor. Methyl ester passes through a reactor bed containing a palladium-based catalyst at a temperature of 135°C and a pressure of 0.3 MPa, and is oxidatively coupled to form dimethyl oxalate with a purity of more than 99%, which is used as a raw material for the subsequent decarbonylation reaction.

[0037] Decarbonylation reaction: take 100g decarbonylation catalyst Na 2 CO 3 Put it in a stainless steel reaction kettle, add 1000g dimethyl oxalate, raise the temperature to 110°C under normal pressure, keep the temperature for 4 hours, take out the liquid phase product after reaction, determine the component composition and content by gas chromatography analysis, and calculate the oxalic acid The conversion rate of dimethyl ester and the selectivity of dimethyl c...

Embodiment 3

[0039] The preparation method of Pd series catalyst is the same as embodiment 1.

[0040] Oxidative coupling reaction: Take 100ml of Pd-based catalyst and place it in the constant temperature zone of the fixed-bed reactor. Methyl ester passes through a reactor bed containing a palladium-based catalyst at a temperature of 150°C and a pressure of 0.5 MPa, and is oxidatively coupled to form dimethyl oxalate with a purity of more than 99%, which is used as a raw material for the subsequent decarbonylation reaction.

[0041] Decarbonylation reaction: take 100g decarbonylation catalyst PPh 4 Cl is placed in a stainless steel reaction kettle, 1000g of dimethyl oxalate is added, the temperature is raised to 140°C under normal pressure, and the temperature is kept at a constant temperature for 5 hours. The conversion rate of dimethyl oxalate and the selectivity of dimethyl carbonate, the results are shown in table 1.

[0042]

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Abstract

The invention discloses a method for indirectly synthesizing dimethyl carbonate by CO gas phase oxidative coupling and decarbonylation. In the process, the reaction conditions are mild, a catalyst is noncorrosive to equipment, and the yield and quality of the dimethyl carbonate are high. The basic raw materials required by the method can be prepared from a carbon resource, so the method is in accordance with the current condition that China has rich coal resource, and has a great significance for reducing dependency on oil resource.

Description

technical field [0001] The invention relates to a preparation method of dimethyl carbonate, in particular to a method for indirectly synthesizing dimethyl carbonate through CO gas-phase oxidative coupling and decarbonylation. Background technique [0002] Dimethyl carbonate is an environmentally friendly organic chemical raw material that meets the requirements of modern "clean technology". It has good reactivity and can replace highly toxic substances such as phosgene, dimethyl sulfate, methyl chloride and methyl chloroformate in many fields. Or carcinogens undergo carbonylation, methylation, methyl esterification and transesterification reactions to generate a variety of important chemical products. Dimethyl carbonate can be used as raw material to synthesize polycarbonate, isocyanate, carbamate and other high value-added fine chemicals. Dimethyl carbonate has excellent solubility and is widely used as a solvent for coatings and pharmaceutical industries. In addition, ...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/00
Inventor 吴晓金张学岭许叶飞吴维果孔国杰
Owner 江苏丹化煤制化学品工程技术有限公司
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