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A zno/sio2-γ-al2o3 catalyzed hydrolysis of methyl bromide to prepare methanol and dimethyl ether

A technology of methyl bromide and catalyst is applied in the field of preparing ZnO/SiO2-γ-Al2O3 catalyst by sol-gel method, which can solve the problems of low conversion rate of methanol or dimethyl ether, poor selectivity and the like, and achieves low reaction temperature, high conversion rate, The effect of the synthesis process is simple

Inactive Publication Date: 2016-06-29
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a ZnO / SiO solution for the existing problems such as low conversion rate or poor selectivity of methanol or dimethyl ether prepared from methyl bromide. 2 -γ-Al 2 o 3 Method for preparing methanol and dimethyl ether by catalytic hydrolysis of methyl bromide

Method used

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  • A zno/sio2-γ-al2o3 catalyzed hydrolysis of methyl bromide to prepare methanol and dimethyl ether
  • A zno/sio2-γ-al2o3 catalyzed hydrolysis of methyl bromide to prepare methanol and dimethyl ether

Examples

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Effect test

Embodiment 1

[0027] γ-Al 2 o 3 Preparation: Weigh 22.5034g of aluminum nitrate nonahydrate and dissolve it in 100ml of water to form a solution in a 250ml beaker. Take 25ml of concentrated ammonia water to dilute 3 times and slowly drop into the solution for making aluminum nitrate. Stir while dripping until the pH of the solution is 8-9, after the precipitation is completed, the slurry is stirred at room temperature for 1 h. Suction filtration was performed and washed until the pH was 7, and the filter cake was dried at 120° C. for 12 hours to obtain a γ-AlOOH precursor. Afterwards, it was calcined in a muffle furnace at 600°C for 4 hours to obtain γ-Al 2 o 3 , grind 180 mesh and sieve for later use.

[0028] 20wt%-ZnO / SiO 2 -γ-Al 2 o 3 Catalyst preparation

[0029]Weigh 3.1680g of oxalic acid solid and dissolve it in 70ml of deionized water to fully dissolve, then add 52.7014g of tetraethyl orthosilicate and seal and stir to form solution A. Weigh 14.6205g of zinc nitrate hexahy...

Embodiment 2

[0034] 10wt%-ZnO / SiO 2 -γ-Al 2 o 3 Catalyst preparation

[0035] Weigh 3.5640g of oxalic acid solid and dissolve it in 70ml of deionized water to fully dissolve, then add 59.2891g of tetraethyl orthosilicate and seal and stir to form solution A. Weigh 7.3103g of zinc nitrate hexahydrate and dissolve it in 10ml of deionized water to obtain solution B. After stirring solution A for 2 hours, add solution B to solution A and add 0.9g of synthesized γ-Al 2 o 3 , continue to stir for 2 hours, then put it in an 80°C water bath and stir until it becomes a solid sol, take it out and pour it into a glass petri dish and place it in a 120°C oven for 6 hours, then take out the dried solid and place it in a muffle furnace at 2°C / min The heating rate is to heat up to 350°C, maintain the temperature for 5 hours and then lower the temperature. After the temperature drops to room temperature, take out the catalyst and sieve out 30-60 mesh for later use. Final 10%-ZnO / SiO 2 -γ-Al 2 o 3 ...

Embodiment 3

[0040] 20wt%-ZnO / SiO 2 -γ-Al 2 o 3 Catalyst preparation

[0041] Weigh 3.1680g of oxalic acid solid and dissolve it in 70ml of deionized water to fully dissolve, then add 52.7014g of tetraethyl orthosilicate and seal and stir to form solution A. Weigh 14.6205g of zinc nitrate hexahydrate and dissolve it in 20ml of deionized water to obtain solution B. After stirring solution A for 2 hours, add solution B to solution A and add 0.8g of synthesized γ-Al 2 o 3 , continue to stir for 2 hours, then put it in an 80°C water bath and stir until it becomes a solid sol, take it out and pour it into a glass petri dish and place it in a 120°C oven for 6 hours, then take out the dried solid and place it in a muffle furnace at 2°C / min The heating rate is to heat up to 350°C, maintain the temperature for 5 hours and then lower the temperature. After the temperature drops to room temperature, take out the catalyst and sieve out 30-60 mesh for later use. Finally get 20%-ZnO / SiO 2 -γ-Al ...

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Abstract

The invention discloses a method for preparing methanol and dimethyl ether by using catalytic hydrolysis of methyl bromide in the presence of ZnO-SiO2-gamma-Al2O3. A catalytic hydrolysis reaction is carried out between methyl bromide and ZnO-SiO2-gamma-Al2O3 under normal pressure, wherein the amount of the catalyst is 3-10g; the reaction temperature is 100 to 260 DEG C; the molar ratio of H2O to CH3Br is 0.5-4; and the concentration CH3Br / N2 of methyl bromide is 0.5-1.2. The method has the advantages of low reaction temperature, low energy consumption and high conversion rate, the selectivity of the methanol and dimethyl ether can be adjusted by changing the reaction conditions, carbon dioxide is not produced, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of functional material preparation and catalytic chemistry research, specifically the preparation of ZnO / SiO by sol-gel method 2 -γ-Al 2 o 3 Catalyst, and methyl bromide is converted into methanol and dimethyl ether on the catalyst, methyl bromide has a higher conversion rate, and does not produce carbon dioxide. Background technique [0002] Supported catalysts are commonly used as industrially produced silica, activated alumina, molecular sieve and silica-alumina, among which silica, alumina and their mixed carriers are used more, according to silica and The existing forms of alumina can be divided into solid solutions, composites and simple mixtures. [0003] Chinese patent CN201080024394.4 discloses a method of preparing alumina and silica materials using aluminum salts, silicic acid, and the like. The process yields both alumina and silica in mixed form. [0004] In CN201080005801.7, a method for preparing a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/06C07C31/04C07C29/124C07C43/04C07C41/16
CPCY02P20/52
Inventor 单永奎占瑛刘玉飞陈正艳姜贤武韩霜霜
Owner EAST CHINA NORMAL UNIV
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