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Catalyst for use in synthesis of methyl formate and preparation method and application thereof

A methyl formate and catalyst technology, which is applied in the field of catalysts and preparations for the synthesis of methyl formate, can solve the problems of catalyst activity loss, catalyst stability not fundamentally improved, and failure to meet catalyst life requirements, etc., to achieve short process , low energy consumption, and simple separation steps

Active Publication Date: 2012-07-25
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the published stability test results show that the stability of the catalyst has not been fundamentally improved, and the catalyst activity will lose about 30% after about 1000 hours, which obviously cannot meet the requirements for catalyst life in industrial production.

Method used

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  • Catalyst for use in synthesis of methyl formate and preparation method and application thereof
  • Catalyst for use in synthesis of methyl formate and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Catalyst preparation process: Weigh copper nitrate 4.0kg, zirconium oxychloride 64.02kg respectively, namely Cu / Zr=1 / 12 (molar ratio), configure mixed salt solution, and press oxalic acid: copper nitrate=0.01mol / Add oxalic acid to the mixed solution at a ratio of mol, and mix well. Potassium hydroxide was used as the precipitating agent, mixed with the mixed solution for precipitation at 70°C under stirring conditions, and then aged for 1 hour. Repeatedly, filter and wash the obtained precipitate to remove soluble heteroions. The resulting filter cake was dried at 60°C for 48h and calcined at 700°C for 1h. Add 0.17kg of potassium bicarbonate to the obtained sample, carefully grind it evenly, and then roast at 450°C for 3 hours to obtain the final catalyst. The catalyst composition (molar ratio) is: Cu / Zr / K=1 / 12 / 0.1.

[0050] (2) Methanol dehydrogenation reaction to generate methyl formate: After molding the catalyst obtained above, it was packed in a fixed-bed r...

Embodiment 2

[0053] (1) Catalyst preparation process: Weigh copper nitrate 8.0kg, zirconium nitrate 3.37kg respectively, namely Cu / Zr=1 / 0.3 (molar ratio), configure mixed salt solution, and press citric acid: copper nitrate=4.0mol / mol Add citric acid to the mixed solution and mix well. Potassium carbonate was used as the precipitating agent, mixed with the mixed solution for precipitation at 60°C under stirring conditions, and then aged for 3 hours. Repeatedly, filter and wash the obtained precipitate to remove soluble heteroions. The resulting filter cake was dried at 80°C for 36h and calcined at 250°C for 8h. Add 13.73 kg of potassium carbonate to the obtained sample, carefully grind it evenly, and then roast it at 350° C. for 3 hours to obtain the final catalyst. The catalyst composition (molar ratio) is: Cu / Zr / K=1 / 0.3 / 6.0.

[0054] (2) Methanol dehydrogenation reaction to generate methyl formate: after molding the catalyst obtained above, it was packed in a fixed-bed reactor to carr...

Embodiment 3

[0056] (1) Catalyst preparation process: Weigh copper nitrate 8kg, zirconium oxynitrate 6.1kg respectively, namely Cu / Zr=1 / 0.8 (molar ratio), configure mixed salt solution, and press malonic acid: copper nitrate=0.08mol / Add malonic acid to the mixed solution at a ratio of mol, and mix well. Using ammonium bicarbonate as a precipitating agent, mix and precipitate with the mixed solution at 80°C under stirring conditions, and then age for 0.5h. Repeatedly, filter and wash the obtained precipitate to remove soluble heteroions. The resulting filter cake was dried at 90°C for 18h and calcined at 500°C for 2h. Add 8.37 kg of potassium nitrate to the obtained sample, grind it carefully and evenly, and then roast it at 450°C for 3 hours to obtain the final catalyst. The catalyst composition (molar ratio) is: Cu / Zr / K=1 / 0.8 / 5.0.

[0057] (2) Methanol dehydrogenation reaction to generate methyl formate: After molding the catalyst obtained above, it was packed in a fixed-bed reactor t...

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Abstract

The invention discloses a catalyst for used in synthesis of methyl formate. The molar ratio of Cu to Zr to K is 1:(0.3-12):(0.1-6). A precipitation method, a co-impregnation method and a stepwise soaking method are adopted for preparing the catalyst. The catalyst has the advantages of high stability and high selectivity of methyl formate.

Description

technical field [0001] The present invention relates to a kind of catalyst and preparation method and application, specifically a kind of catalyst for synthesizing methyl formate, preparation method and application. technical background [0002] Methyl formate is an important chemical intermediate. Starting from methyl formate, important chemicals such as formic acid, formamide, dimethylformamide, dimethyl carbonate, and ethylene glycol can be produced. At present, the methanol carbonylation route is often used in industrial production, but this method requires a large investment in equipment, high cost of refining raw materials, catalyst separation problems in the process, and high cost of disposal of the formed organic salt residue. Chinese patent CN1064672C discloses a continuous preparation method of methyl formate, which aims to reduce the generation of organic salts and reduce the processing cost of distillation residues by increasing the reaction pressure and temperat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78C07C69/06C07C67/39
Inventor 李德宝陈从标肖勇
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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