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Double-micropore zeolites and method of making thereof

A microporous zeolite and microporous technology, which is applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problem that the amount of added aluminum source and alkali is difficult to grasp, and the repeatability of synthesizing double microporous molecular sieve is not easy. control and other issues, to achieve good thermal and hydrothermal stability, strong acidity, and the effect of improving Si/Al ratio

Inactive Publication Date: 2009-10-21
TAIYUAN UNIV OF TECH
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Our research group adopted two-step crystallization and successfully prepared a double-microporous molecular sieve (patent authorization number: ZL200410012333.2) that organically combines Y and Beta zeolites. It is characterized in that the zeolite synthesized in the first step is used as the second During the two-step synthesis of raw materials, it is required to pour part of the clear liquid. Since the clear liquid contains silicon, aluminum, alkali and other components, it is difficult to control the amount of aluminum source and alkali added in the second step of synthesis, resulting in the synthesis of double micropores. The repeatability of molecular sieve is not easy to control

Method used

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  • Double-micropore zeolites and method of making thereof

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Experimental program
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Effect test

Embodiment approach 1

[0018] Step 1: Mix 17.4g TEABr (tetraethylammonium bromide), 6ml concentrated ammonia water, 2.26g sodium metaaluminate, 0.5g NaOH, 31ml silica sol, and 34ml distilled water to form a uniform white jelly, and put it into 100ml stainless steel In the reaction kettle, crystallize at 140°C for 10 days and take it out for use. The molar ratio of the original material of Beta zeolite is: 2.2Na 2 O: 20SiO 2 :Al 2 o 3 : 4.6 (TEA) 2 O: 4.6 (NH 4 ) 2 O: 440H 2 O.

[0019] The second step: Add 2.35g sodium metaaluminate, 1.31g sodium hydroxide, and 2.5mlY directing agent to the solid-liquid mixture containing Beta zeolite synthesized above, and the total molar ratio of materials is: 2.62Na 2 O:Al 2 o 3 : 9.7SiO2 2 : 2.32 (TEA) 2 O: 2.32 (NH 4 ) 2 O: 215H 2 O. Then mix and stir evenly, put it into a 100ml stainless steel reaction kettle, crystallize at 85°C for 24h, take it out, then cool it with tap water at room temperature, then wash it with distilled water until neutra...

Embodiment approach 2

[0021]Step 1: Mix 17.4g TEABr (tetraethylammonium bromide), 6ml concentrated ammonia water, 2.26g sodium metaaluminate, 0.5g NaOH, 31ml silica sol, and 34ml distilled water to form a uniform white jelly, and put it into 100ml stainless steel In the reaction kettle, crystallize at 145°C for 8 days and take it out for use. The molar ratio of the original material of Beta zeolite is: 2.2Na 2 O: 20SiO 2 :Al 2 o 3 : 4.6 (TEA) 2 O: 4.6 (NH 4 ) 2 O: 440H 2 O.

[0022] The second step: Add 2.97g sodium metaaluminate, 1.31g sodium hydroxide, and 3.5mlY directing agent to the solid-liquid mixture containing Beta zeolite synthesized above, and the total material molar ratio is: 2.47Na 2 O:Al 2 o 3 : 8.55 SiO 2 : 2.04 (TEA) 2 O: 2.04 (NH 4 ) 2 O: 190H 2 O. Mix and stir to form a uniform white substance, put it into a 100ml stainless steel reaction kettle, crystallize at 90°C for 24 hours, take it out, then cool it with tap water at room temperature, then wash it with distil...

Embodiment approach 3

[0024] Step 1: Mix 17.4g TEABr (tetraethylammonium bromide), 6ml concentrated ammonia water, 2.26g sodium metaaluminate, 0.5g NaOH, 31ml silica sol, and 34ml distilled water to form a uniform white jelly, and put it into 100ml stainless steel In the reaction kettle, crystallize at 135°C for 13 days and take it out for use. The molar ratio of the original material of Beta zeolite is: 2.2Na 2 O: 20SiO 2 :Al 2 o 3 : 4.6 (TEA) 2 O: 4.6 (NH 4 ) 2 O: 440H 2 O.

[0025] The second step: Add 3.15g sodium metaaluminate, 1.07g sodium hydroxide, and 3.5mlY directing agent to the solid-liquid mixture containing Beta zeolite synthesized above, and the total material molar ratio is: 2.30 Na 2 O:Al 2 o 3 : 8.27 SiO 2 : 1.98 (TEA) 2 O: 1.98 (NH 4 ) 2 O: 184H 2 O. Mix and stir to form a uniform white substance, put it into a 100ml stainless steel reaction kettle, crystallize at 90°C for 24 hours, take it out, then cool it with tap water at room temperature, then wash it with dis...

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Abstract

A kind of double microporous zeolite and preparation method thereof belong to the technical field of fine chemical industry, it is characterized in that adopting two-step crystallization method, the first step first synthesizes Beta, then with the synthetic Beta reaction mixture as the raw material of the second step synthesizing Y zeolite, The composite zeolite product with BEA / FAU structure is obtained by supplementing the aluminum source, adjusting the basicity of the system, adding the directing agent for synthesizing Y zeolite for reaction crystallization, filtering, washing, drying, and calcining. The method successfully solves the problems of pouring part of the clear liquid and difficult control of the amount of aluminum source and base added in the synthesis because the clear liquid contains components such as silicon, aluminum and alkali, and the product repeatability is difficult to control. The synthesized Beta / Y composite zeolite products can be used as various catalysts, catalyst assistants and adsorbents. After ion exchange, they have strong acidity and good thermal and hydrothermal stability. They can be used as various catalysts, catalyst assistants It is bound to have potential application value in catalytic cracking and hydrocracking of petrochemical industry.

Description

1. Technical field [0001] The invention relates to a double-microporous zeolite and a preparation method thereof, which belong to the technical field of fine chemicals, and specifically relate to a two-step crystallization method to organically combine two microporous zeolites of Beta and Y to form a double-microporous zeolite. A technical solution for a new type of zeolite material with a microporous structure. 2. Technical background [0002] Y-type molecular sieves and their modified products show excellent catalytic performance in reactions such as catalytic cracking, hydrocracking, hydroisomerization, alkane aromatization, and alkylation (M.A.Saberi, R.Le Van Mao, M.A. . Martin, A.W.H. Mak. Applicd Catalysis A: General 214 (2001); I.P. Dzikh, J.M. Lopes, F. Lemos, F. Ribeiro.CatalysisToday 65(2001); Wei Ruiping, Wang Jun, Ren Xiaoqian, etc. Journal of Inorganic Chemistry. 12(2004); A.M.Radwan, zhang-GuoZhang, P.Chambrion, et al.Fuel Processing Technology 55(1998).), i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/06B01J29/08
Inventor 李瑞丰郑家军张喜文郭群于峰凌凤香马静红孙万付
Owner TAIYUAN UNIV OF TECH
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