Method for preparing ZSM-34 and heteroatom substituted molecular sieve thereof by using crystal seed synthesis method

A technology of molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of long crystallization time and achieve the effects of reducing crystallization time, good crystallinity and purity, and environmental friendliness

Inactive Publication Date: 2011-02-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, Xiao Fengshou and others successfully synthesized ZSM-34 (CN Patent No.200710056022.X.) using L-directing agent without organic template. Although the cost is reduced, it is necessary to prepare L-directing agent and aluminum sulfate soluti

Method used

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  • Method for preparing ZSM-34 and heteroatom substituted molecular sieve thereof by using crystal seed synthesis method
  • Method for preparing ZSM-34 and heteroatom substituted molecular sieve thereof by using crystal seed synthesis method
  • Method for preparing ZSM-34 and heteroatom substituted molecular sieve thereof by using crystal seed synthesis method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Synthesis of ZSM-34 zeolite molecular sieve by seed crystal method

[0023] First, the 14.7gH 2 O mixed with 0.36g aluminum sulfate, then added 0.242gKOH, 0.795gNaOH, then added 1.75g ​​white carbon black under stirring, continued stirring until the solution became uniform, then added 3%

[0024] ZSM-34 molecular sieve is used as crystal seed (the amount of seed crystal is based on the input SiO 2 mass percent calculation). Add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallize at 140°C for 8 hours to complete the crystallization, filter the product with suction, and dry it to obtain the product. The proportioning of reaction raw material is as follows:

[0025] SiO 2 : 0.019Al 2 o 3 : 0.328Na 2 O: 0.064K 2 O: 27.6H 2 O. The mass ratio of seed crystal to white carbon black is 3%.

[0026] Its structure is ZSM-34 zeolite molecular sieve through X-ray diffraction analysis, and it can be seen from ...

Embodiment 2

[0028] Embodiment 2: Secondary utilization of the product prepared by the seed crystal method

[0029] 14.7gH 2 O and 0.36g of aluminum sulfate are mixed evenly, then add 0.242gKOH, 0.795gNaOH to it, then add 1.75g ​​of white carbon black under stirring, continue stirring until the solution becomes uniform, then add 3% of ZSM-34 synthesized in Example 1 Molecular sieves were used as crystal seeds, and after stirring evenly, the gel was added into a polytetrafluoroethylene stainless steel reaction kettle, and crystallized in an oven at 140°C for 8 hours. The product was filtered with suction and dried.

[0030] attached figure 2 The XRD spectrum of the product synthesized by the reuse of the ZSM-34 zeolite molecular sieve prepared by the seed crystal method, it can be seen from the spectrum that the product has a typical ZSM-34 zeolite molecular sieve structure, and the sample has a relatively high degree of crystallinity.

[0031] attached image 3 The scanning electron m...

Embodiment 3

[0032] Example 3: Using KNO 3 Replace KOH as potassium source

[0033] 14.7gH 2 O mixed with 0.36g aluminum sulfate, add 0.36g KNO 3 Finally, add 0.95gNaOH again, then add 1.75g ​​white carbon black under stirring, continue to stir until after the solution becomes uniform, add 3% ZSM-34 molecular sieve to do crystal seed (the amount of seed crystal is based on the percentage of input SiO 2mass percent calculation). Add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallize at 140°C for 8 hours to complete the crystallization, filter the product with suction, and dry it to obtain the product.

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Abstract

The invention relates to a molecular sieve preparation method, in particular to a method for synthesizing a ZSM-35 molecular sieve by using a crystal seed method. The method comprises the following steps of: uniformly mixing deionized water and an aluminum source together, adding a potassium source and NaOH, adding white carbon black while stirring, continuously stirring until the solution is uniform and becomes silica-alumina gel, adding a ZSM-35 molecular sieve crystal seed into the silica-alumina gel, and stirring; placing the mixture in a reaction kettle, crystallizing for 3 hours to 5 days at 100-180 DEG C, or crystallizing for 1-10 days at 70-100 DEG C; filtering the product by suction, and drying to obtain the ZSM-34 molecular sieve. The method not only maintains good crystallinity and purity, but also has good catalytic reaction activity. The entire production process not only does not use any organic template agents, but also can greatly shorten crystallization time by using the crystal seed method. Thus, unnecessary loss in the production process is reduced, the product also has larger specific surface area, and the product has potential application value to certain important catalytic reactions. The inorganic raw materials adopted during product are all friendly to environment and cheap.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for preparing ZSM-34 and heteroatom-substituted molecular sieves by a seed crystal synthesis method. Background technique [0002] Because of its open structure and large surface area, molecular sieves are widely used in many fields, such as ion exchange, adsorption and separation, host-guest chemistry, etc., and have been widely used in petrochemical and fine chemical industries. Rubin et al first used ((CH 3 ) 3 NCH 2 CH 2 OH) as a template to synthesize ZSM-34 molecular sieve (USP4,086,186). ZSM-34 is a zeolite (8-membered ring Channels and 12-membered rings channels crossed) and erionite (three-dimensional 8-membered ring A symbiont of the channel). Because of its good catalytic activity and selectivity in the methanol conversion reaction (MTO), it has aroused great interest of researchers. [0003] Since the synthesis of ZSM-34 zeolite molecular ...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/06
Inventor 肖丰收杨承广张琳孟祥举
Owner ZHEJIANG UNIV
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