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Method for preparing Cu-Ni diatom doped mesoporous molecular sieve catalyst

A mesoporous molecular sieve and catalyst technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low hydrothermal stability, low catalyst efficiency, weak acidity, etc. Highly reactive effect

Inactive Publication Date: 2016-01-27
QINGDAO LANNONGGU AGRI PROD RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It solves the problems of low catalyst efficiency, weak acidity and low hydrothermal stability of hydrothermally synthesized mesoporous molecular materials in the process of methanol, carbon dioxide and DMC.

Method used

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  • Method for preparing Cu-Ni diatom doped mesoporous molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Add 0.3g of sodium metaaluminate, 8.0g of silicon dioxide (30%), 0.25g of water glass, 0.2g of copper sulfate and 0.1g of nickel sulfate into the autoclave, stir well, and then crystallize at 100°C for 4h. Then add 2gEO20PO70EO20 (P123) and 15g acid functionalized ionic liquid therein. Stir at 40°C for 20h. Then control the crystallization conditions (95°C, 23 hours) to adjust the size and purity of the crystal form. The obtained crystals are sequentially filtered under reduced pressure, washed with ultrapure water, washed with ethanol and dried in vacuum to obtain the original powder of the mesoporous molecular sieve. Finally, the raw powder was calcined in a muffle furnace at 450° C. for 6 hours to obtain a catalyst, which is designated as Catalyst 1.

Embodiment 2

[0019] Example 2: Add 0.7g of sodium metaaluminate, 8.0g of silicon dioxide (30%), 0.25g of water glass, 0.5g of copper sulfate and 0.3g of nickel sulfate into the autoclave, stir evenly, and crystallize at 100-140°C 4h. Then 8gEO20PO70EO20(P123) and 23g acid-functionalized ionic liquid were added to it. Stir at 40°C for 20h. Then control the crystallization conditions (95°C, 23 hours) to adjust the size and purity of the crystal form. The obtained crystals are sequentially filtered under reduced pressure, washed with ultrapure water, washed with ethanol and dried in vacuum to obtain the original powder of the mesoporous molecular sieve. Finally, the raw powder was calcined in a muffle furnace at 550° C. for 6 hours to obtain a catalyst, which is designated as Catalyst 2.

Embodiment 3

[0020] Example 3: Add 0.5g of sodium metaaluminate, 6.0g of silicon dioxide (30%), 0.45g of water glass, 0.3g of copper sulfate and 0.3g of nickel sulfate into the autoclave, stir well, and crystallize at 120°C for 4h . Then add 5gEO20PO70EO20 (P123) and 19g acid functionalized ionic liquid thereinto. Stir at 40°C for 20h. Then control the crystallization conditions (95°C, 23 hours) to adjust the size and purity of the crystal form. The obtained crystals are sequentially filtered under reduced pressure, washed with ultrapure water, washed with ethanol and dried in vacuum to obtain the original powder of the mesoporous molecular sieve. Finally, the raw powder was calcined in a muffle furnace at 500° C. for 6 hours to obtain a catalyst, which is designated as Catalyst 3 .

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Abstract

The present invention discloses a method for preparing a Cu-Ni diatom doped mesoporous molecular sieve catalyst. The Cu-Ni diatom doped mesoporous molecular sieve catalyst is prepared by ion thermal synthesis method. First, sodium metaaluminate, silica, water glass, copper sulfate and nickel sulfate are evenly mixed in a high pressure reactor, and then crystallized at 100-140 DEG C for 4h; subsequently, EO20PO70EO20 (P123) is added into the high pressure reactor, an acid functional ionic liquid is used as a template agent for stirring for 20h at constant temperature of 40 DEG C, mesoporous molecular sieve product raw powder is obtained by crystallization, filtration, washing and drying and other processes; finally, the raw powder is calcined in a muffle furnace for 6 hours at 450-550 DEG C to obtain the catalyst. The Cu-Ni diatom doped mesoporous molecular sieve catalyst prepared by the ion thermal synthesis method has high reactivity, good stability and other characteristics in a carbon dioxide ethanol reaction vessel, meanwhile by use of the catalyst, the methanol conversion rate is over 20%, and the DMC selectivity is 95% or more.

Description

technical field [0001] The invention relates to the field of preparation of mesoporous molecular sieve materials, in particular to a method for preparing a mesoporous molecular sieve catalyst doped with Cu-Ni diatoms. Background technique [0002] Dimethyl carbonate (DMC) is known as the "new cornerstone" of organic synthesis today, and is widely used in the production process of synthetic dyes, medicines, pesticides, dyes, lubricating oil additives, food additives, etc. Using methanol and carbon dioxide as raw materials is the main method for synthesizing DMC. On the one hand, this method solves the emission of greenhouse gas CO2, and on the other hand, it turns waste into treasure. However, the conversion of the process is too low due to the difficult activation of CO2. In order to improve the conversion efficiency of this process, researchers at home and abroad have done a lot of research on high-efficiency catalyst methods. In particular, the development of metal-suppo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/072C07C68/04C07C69/96
CPCY02P20/141
Inventor 宋波
Owner QINGDAO LANNONGGU AGRI PROD RES & DEV