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Method for preparing methanol synthesizing catalyst

A technology for synthesizing methanol and catalysts, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of easy deactivation of catalysts and achieve improved methanol performance, uniform particle size distribution, and high density. Effect

Inactive Publication Date: 2009-11-25
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To solve the problem that the catalyst is easily deactivated in the slurry bed and fixed bed

Method used

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  • Method for preparing methanol synthesizing catalyst

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Embodiment 1

[0016] The copper / zinc / aluminum mol ratio that preparation concentration is 1.5mol / L is the mixed nitrate solution of 64 / 32 / 4 and the sodium carbonate solution that concentration is 1.3mol / L respectively 500ml, under 80 ℃ and fully stirring condition, And keep the pH of the precipitation mother liquid in the range of 8.0±0.2, carry out the precipitation reaction in a constant temperature water bath, after the precipitation is completed, continue to stir and age under microwave radiation at 90°C for 2 hours, and then wash the precipitated product with deionized water until it is sodium-free Until the ions are detected, dry in an oven at 110°C for 11 hours, and finally bake in an air atmosphere at 320°C for 3 hours. The methanol synthesis reaction is carried out in a mechanically stirred slurry bed reactor with a volume of 500ml, and the reaction conditions are 240°C of temperature, 4MPa of pressure, (H 2 -CO 2 ) / (CO+CO 2 )=2, air speed 1600L / kg cat h. The results obtained a...

Embodiment 2

[0018] The copper / zinc / aluminum mol ratio that preparation concentration is 1.5mol / L is the mixed nitrate solution of 64 / 32 / 4 and the sodium carbonate solution that concentration is 1.3mol / L respectively 500ml, under 80 ℃ and fully stirring condition, And keep the pH of the precipitation mother liquid in the range of 8.0±0.2, carry out the precipitation reaction in the microwave, after the precipitation is completed, age it in a constant temperature water bath at a temperature of 80°C and continue to stir for 1 hour, and then wash the precipitated product with deionized water until it is free Until the sodium ion is detected, dry it in an oven for 11 hours, and finally bake it in a muffle furnace at 350°C for 1 hour in an air atmosphere. The methanol synthesis reaction is carried out in a mechanically stirred slurry bed reactor with a volume of 500ml, and the reaction conditions are 240°C of temperature, 5.0MPa of pressure, (H 2 -CO 2 ) / (CO+CO 2 )=2, air speed 800L / kg cat h...

Embodiment 3

[0020] Prepare 1.5mol / L copper / zinc / aluminum mixed nitrate solution with a molar ratio of 64 / 32 / 4 and 1.3mol / L sodium carbonate solution with a concentration of 500ml respectively. , and keep the pH of the precipitation mother liquid in the range of 7.5±0.2, carry out the precipitation reaction, after the precipitation is completed, age in a constant temperature water bath at 60°C and continue to stir for 3 hours, and then wash the precipitated product with deionized water until it is free of sodium ions. Dry the filter cake in a microwave oven at 110°C for 3 hours, and finally bake it in a microwave oven at 370°C for 1 hour in an air atmosphere. The methanol synthesis reaction is carried out in a mechanically stirred slurry bed reactor with a volume of 500ml, and the reaction conditions are 240°C of temperature, 5.0MPa of pressure, (H 2 -CO 2 ) / (CO+CO 2 )=1.5, air speed 2000L / kg cat h. The reaction results are shown in Table 1.

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Abstract

According to a method for preparing methanol synthesizing catalyst, a water solution which contains copper nitrate, zinc nitrate, aluminum nitrate and a fourth component with a total concentration of 0.5-2.0mol / L and a water solution that contains the sodium carbonate with a concentration of 0.5-2mol / L are prepared. At a state that the temperature is controlled to 50-80 DEG C with the microwave, the pH value is controlled to 6.5-8.5 for executing coprecipitation reaction. Then the water solution is aged for 0.5-3 hours in the temperature of 60-90 DEG C, which is controlled with the microwave. Then the precipitate is washed and filtered with the de-ionized water. Then the filter cake is dried for 1-11 hours at the condition that the temperature is controlled to 70-150 DEG C with the microwave. Finally the dried precipitate is calcined for 1-5 hours at the condition that the temperature is controlled to 300-400 DEG C with the microwave for obtaining the target catalyst. The method of the invention has the advantages of simple technique, moderate operation condition, smaller and more uniform catalyst particle particularly when the microwave heating is introduced and higher mechanical strength of the catalyst. The test through the static bed and the slurry-bed reactor shows that the activity and the stability of the catalyst are better than those of the catalyst prepared through the conventional heating and the bottleneck of incapability for industrializing of the slurry-bed caused by the easy inactivation is broken through.

Description

technical field [0001] A method for preparing a catalyst for synthesizing methanol, especially a method for preparing a catalyst for synthesizing methanol which includes at least one step of introducing microwave radiation in the process of precipitation, aging, drying and roasting. technical background [0002] Methanol is an extremely important chemical raw material, a green liquid fuel and an excellent heat carrier. Therefore, the development and application of catalysts for the synthesis of methanol have always been concerned. There are three main types of existing methanol catalysts, namely: copper-based catalysts, non-copper-based catalysts and liquid-phase methanol catalysts. Among them, copper-based catalysts have the characteristics of mild operating conditions, high activity and high stability, and are widely used and promoted in industry. In order to improve the performance of copper-based catalysts for catalytic synthesis of methanol, researchers have studied a...

Claims

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Application Information

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IPC IPC(8): B01J23/80B01J37/34B01J23/889B01J23/887B01J23/847C07C31/04C07C29/154C07C29/156
CPCY02P20/52
Inventor 李忠范辉郑华艳郭启海刘岩张小兵
Owner TAIYUAN UNIV OF TECH
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