Method for synthesizing aluminum-rich * MRE zeolite molecular sieve in one step by using organic template agent

A technology of zeolite molecular sieve and organic template agent, which is applied in the direction of crystalline aluminosilicate zeolite, molecular sieve and alkali exchange compound, chemical instrument and method, etc., can solve the problem of increasing the cost of synthesizing ZSM-48 zeolite molecular sieve, hexamethylene bromide The high cost of diammonium and the high price of crown ether have achieved the effect of easy-to-obtain structure, excellent guiding performance, and low silicon-aluminum ratio

Active Publication Date: 2020-08-25
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN103803576B discloses a method of using crown ether (12-crown ether-4) as a template and ZSM-48 as a seed crystal to synthesize a ZSM-48 zeolite molecular sieve with a silicon-aluminum ratio of 30-50, but the price of crown ether is very high. expensive and expensive
CN110562999A discloses a method of using hexamethylene bromide bisammonium bromide as an organic template and zeolite molecular sieve as the crystal seed to synthesize ZSM-48 with a silicon-aluminum ratio of 40-100, but the hexamethylene bromide used in the method The high cost of diammonium
CN110342536A discloses a method for synthesizing a ZSM-48 zeolite molecular sieve with a silicon-aluminum ratio of 30-600 with a double-template agent, but using a double-template agent in the synthesis system increases the cost of synthesizing the ZSM-48 zeolite molecular sieve

Method used

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  • Method for synthesizing aluminum-rich * MRE zeolite molecular sieve in one step by using organic template agent
  • Method for synthesizing aluminum-rich * MRE zeolite molecular sieve in one step by using organic template agent

Examples

Experimental program
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Effect test

Embodiment 1

[0028] First, add 1.73g of tetraethoxysilane to 4g of diethyldimethylammonium hydroxide aqueous solution and 3.6g of deionized water, then add 0.113g of aluminum isopropoxide, and finally add 0.05g of sodium chloride and stir After 12 hours, add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, and crystallize at 180°C for 48 hours to complete the crystallization. After the reaction is completed, the reaction product is washed with deionized water and dried at 80°C for 12 hours to obtain Al-rich* MRE zeolite molecular sieve.

[0029] The molar ratio of the reaction raw materials is as follows: SiO 2 :Al 2 o 3 : Na 2 O: R: H 2 O=30:1:1.5:30:1200.

[0030] Its structure is *MRE zeolite molecular sieve ( figure 1 ), and it can be seen from the scanning electron microscope that the length of the synthesized product is 1 μm, and the width is about 100 nm in a one-dimensional rod-like structure ( figure 2 ). The ICP assay results of ...

Embodiment 2

[0032] The addition sequence and stirring time of gel preparation are the same as in Example 1, and the amount of each material is 1.73g of tetraethoxysilane, 4g of diethyldimethylammonium hydroxide aqueous solution, 3.6g of deionized water, and 0.05g of sodium chloride , 0.057g of aluminum isopropoxide, crystallized at 180°C for 48h, and then completely crystallized. After the reaction was completed, the reaction product was washed with deionized water and dried at 80°C for 12h to obtain an aluminum-rich *MRE zeolite molecular sieve.

[0033] The molar ratio of the reaction raw materials is as follows: SiO 2 :Al 2 o 3 : Na 2 O: R: H 2 O=30:0.5:1.5:30:1500.

Embodiment 3

[0035] The addition sequence and stirring time of gel preparation are the same as Example 1, and the amount of each material is 1.73g of tetraethoxysilane, 4g of diethyldimethylammonium hydroxide aqueous solution, 3.6g of deionized water, and 0.05g of sodium chloride , 0.17g of aluminum isopropoxide, crystallized at 180°C for 48h to complete crystallization, after the reaction was completed, the reaction product was washed with deionized water and dried at 80°C for 12h to obtain an aluminum-rich *MRE zeolite molecular sieve.

[0036] The molar ratio of the reaction raw materials is as follows: SiO 2 :Al 2 o 3 : Na 2 O: R: H 2 O=30:1.5:1.5:30:1500.

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Abstract

The invention relates to the field of preparation of zeolite molecular sieves, and aims to provide a method for synthesizing an aluminum-rich * MRE zeolite molecular sieve in one step by using an organic template agent. The method comprises the following steps: firstly, mixing a silicon source with deionized water and a diethyldimethylammonium hydroxide aqueous solution, then adding an aluminum source, and finally adding solid sodium salt and potassium salt; fully stirring for 12 hours and then putting the mixture into a reaction kettle; and carrying out a crystallization reaction at 160-200 DEG C for 24-168 h, washing the reaction product with deionized water, and drying the reaction product at 80 DEG C for at least 12 h to obtain the aluminum-rich * MRE zeolite molecular sieve. Accordingto the invention, cheap diethyldimethylammonium hydroxide is used as an organic template agent to synthesize the aluminum-rich * MRE zeolite molecular sieve in one step, the crystallization time is short, and the method has important significance in the field of actual chemical production. The minimum silica-alumina ratio of the obtained aluminum-rich * MRE zeolite molecular sieve can reach 19.2,so that enough acid strength can be provided for the reaction.

Description

technical field [0001] The invention relates to the field of preparation of zeolite molecular sieves, in particular to a method for synthesizing aluminum-rich * MRE zeolite molecular sieves in one step with an organic template. Background technique [0002] Zeolite molecular sieve materials are widely used in petrochemical, fine chemistry, and environmental protection fields due to their large specific surface area, rich acid sites, uniform micropore distribution, and excellent thermal and hydrothermal stability. One-dimensional zeolite molecular sieve materials such as TON zeolite molecular sieve have a good catalytic effect in the hydroisomerization reaction of alkanes. The hydroisomerization reaction of linear alkanes is one of the important improvements in the refining process, which can not only reduce the pour point of oil, but also maintain the yield and high viscosity of oil, and greatly improve the quality of oil products. [0003] *MRE zeolite molecular sieve also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/04
CPCC01B39/04C01B39/48C01P2002/72C01P2004/03
Inventor 吴勤明洪鑫孟祥举肖丰收
Owner ZHEJIANG UNIV
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