Micro-mesoporous structure beta-molecular sieve, Ni-based micro-mesoporous beta-molecular sieve catalyst and preparation method thereof

A molecular sieve and catalyst technology, used in molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc., can solve the problems of single pore structure of microporous Beta molecular sieve, uneven distribution of catalyst active components, and small specific surface area. Simple operation steps, good hydrothermal stability, stable molecular structure effect

Inactive Publication Date: 2019-01-18
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention solves the problems of single pore structure, small specific surface area, uneven distribution of catalyst active components and low catalytic efficiency in existing microporous Beta molecular sieves, and provides a micro-media with high crystallinity, large specific surface area and good pore connectivity. Porous Beta molecular sieve and its preparation method, its unique skeleton structure and excellent physical and chemical properties make it a

Method used

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  • Micro-mesoporous structure beta-molecular sieve, Ni-based micro-mesoporous beta-molecular sieve catalyst and preparation method thereof
  • Micro-mesoporous structure beta-molecular sieve, Ni-based micro-mesoporous beta-molecular sieve catalyst and preparation method thereof
  • Micro-mesoporous structure beta-molecular sieve, Ni-based micro-mesoporous beta-molecular sieve catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: Micro-mesoporous Beta molecular sieve preparation method, comprises the following operation steps:

[0028] One, the tetraethylammonium hydroxide C of content 25% 8 h 21 Add 23.50ml of NO aqueous solution, 19ml of deionized water, and 3ml of sodium hydroxide solution with a concentration of 8mol / L, and stir evenly;

[0029] 2. At 25°C, add a mixture of acetonitrile and toluene with a volume ratio of 1:1 into a three-necked flask, heat the reaction to 75°C, and measure 0.005mol of bromooctadecane and 0.0025mol of N,N,N' ,N'-Tetramethyl-1,6-hexanediamine was added dropwise to the mixed solution in sequence, and continued to reflux and stir at the above temperature for 15 hours; After the organic solvent in the flask was rotary evaporated, the reaction product in the flask was dissolved in ethyl acetate, washed and filtered repeatedly, and finally the product was dried overnight in a vacuum oven at 48°C, and the product obtained after drying and grinding wa...

Embodiment 2

[0041] Embodiment 2: the preparation method of micro-mesoporous Beta molecular sieve, comprises the following operation steps:

[0042] One, the tetraethylammonium hydroxide C of content 25% 8 h 21 Add 23.00ml of NO aqueous solution, 18.5ml of deionized water, and 3.20ml of sodium hydroxide solution with a concentration of 8mol / L, and stir evenly;

[0043] 2. At 30°C, add a mixture of acetonitrile and toluene with a volume ratio of 1:1 into the three-necked flask, heat the reaction to 70°C, and measure 0.005mol of bromooctadecane and 0.0025mol of N,N,N' , N'-tetramethyl-1,6-hexanediamine was added dropwise to the mixed solution in sequence, and continued to reflux and stir at the above temperature for 15 hours; After the organic solvent in the flask was rotary evaporated, the reaction product in the flask was dissolved in ethyl acetate, washed and filtered repeatedly, and finally the product was dried overnight in a vacuum oven at 40°C, and the product obtained after drying ...

Embodiment 3

[0055] Embodiment 3: preparation method of micro-mesoporous Beta molecular sieve, comprises the following steps:

[0056] One, the tetraethylammonium hydroxide C of content 25% 8 h 21 Add 24.0ml of NO aqueous solution, 19.5ml of deionized water, and 2.8ml of sodium hydroxide solution with a concentration of 8mol / L, and stir evenly;

[0057] 2. At 28°C, add a mixture of acetonitrile and toluene with a volume ratio of 1:1 into the three-necked flask, heat the reaction to 72°C, and measure 0.005mol of bromooctadecane and 0.0025mol of N,N,N' , N'-tetramethyl-1,6-hexanediamine was added dropwise to the mixed solution in turn, and continued to reflux and stir at the above temperature for 15 hours; After the organic solvent in the flask was rotary evaporated, the reaction product in the flask was dissolved in ethyl acetate, washed and filtered repeatedly, and finally the product was dried overnight in a vacuum oven at 50°C, and the product obtained after drying and grinding was Te...

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Abstract

The invention relates to a molecular sieve and a catalyst, in particular to a micro-mesoporous structure beta-molecular sieve, an Ni-based micro-mesoporous beta-molecular sieve catalyst and a preparation method thereof. The micro-mesoporous structure beta-molecular sieve solves the problems of narrow pore passage and small specific surface area of the existing microporous Beta molecular sieve andthe problems of diffusion limitation of an Ni-based molecular sieve catalyst. The method comprises the following steps of preparing a template agent C18-6-18Br2 through reaction between bromooctadecane and N,N,N',N'-tetramethyl-1,6-hexamethylene diamine according to the mol ratio of 2:1 in acetonitrile and toluol (1:1 v/v); then, performing hydro-thermal synthesis of the micro-mesoporous beta-molecular sieve by tetra-ethylalnmonium hydroxide water solution, the template agent and other chemical raw materials; next, loading nickel nitrate hexahydrate onto the molecular sieve to obtain the Ni-based micro-mesoporous beta-molecular sieve catalyst. The method has the advantages that the self made template agent is used for synthesizing the micro-mesoporous beta-molecular sieve; the cost is low;the synthesized micro-mesoporous beta-molecular sieve has good pore passage communication performance; by using the prepared Ni-based micro-mesoporous beta-molecular sieve catalyst, the ethanol conversion rate and hydrogen gas selectivity are obviously improved.

Description

technical field [0001] The invention relates to a molecular sieve and a catalyst, in particular to a micro-mesoporous Beta molecular sieve, a Ni-based micro-mesoporous Beta molecular sieve catalyst and a preparation method thereof. Background technique [0002] In recent years, coal, oil, natural gas and other non-renewable energy sources have been consumed in large quantities. Human beings are facing serious energy crises and environmental problems. Finding new alternative energy sources is an urgent problem to be solved. Hydrogen energy has attracted widespread attention due to its renewable, non-polluting combustion, and wide-ranging sources. Among them, indirect hydrogen production from biomass ethanol is considered to be the most economically feasible way. Therefore, the selection of suitable catalyst supports and transition metals with strong C-C bond and C-H bond breaking ability is the key to improve ethanol conversion and hydrogen selectivity. Beta molecular sieve...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/76B01J35/10B01J37/08B01J37/03C01B3/22
CPCB01J29/7615B01J35/109B01J37/0018B01J37/031B01J2229/18C01B3/22C01B39/04C01B2203/1082C01B2203/1229
Inventor 田韧谢鲜梅王诗瑶
Owner TAIYUAN UNIV OF TECH
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