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Method for synthesis of high silicon zeolite molecular sieve with universal gel

A high-silica zeolite and molecular sieve technology, which is applied in the directions of crystalline aluminosilicate zeolite, iron conglomerate crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the serious discharge of waste liquid and exhaust gas. , high synthesis cost, high toxicity and other problems, to achieve the effect of reducing loss, good crystallinity and purity, and low price

Inactive Publication Date: 2017-03-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of these organic templates has many disadvantages: high synthesis cost, high toxicity, serious waste liquid and exhaust gas emissions
However, they did not start from the most basic structural units (four-membered ring, five-membered ring, six-membered ring) to discuss the synthesis of zeolite molecular sieves

Method used

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  • Method for synthesis of high silicon zeolite molecular sieve with universal gel
  • Method for synthesis of high silicon zeolite molecular sieve with universal gel
  • Method for synthesis of high silicon zeolite molecular sieve with universal gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Crystallization of universal precursor at 160°C

[0027] First, the 8.12gH 2 O (deionized water, the same below) and 0.092g of aluminum sulfate are mixed uniformly, then 0.38g of NaOH is added thereto, and then 3.32g of silica sol (silicon dioxide content 30.5%, the same below) is added under stirring, and the stirring is continued until the solution becomes uniform, then add the reaction raw materials into a polytetrafluoroethylene stainless steel reactor, crystallize at 160°C for 24 hours, filter the product with suction, and dry it to obtain the product.

[0028] The ratio of the reaction raw materials is as follows: SiO 2 :0.0083Al 2 o 3 :0.28Na 2 O:35H 2 o

[0029] Its structure is amorphous by X-ray diffraction analysis. attached figure 1 It is the XRD spectrum of the universal precursor after crystallization at 160°C.

Embodiment 2

[0030] Example 2: Crystallization of the universal precursor with the addition of ZSM-5 zeolite molecular sieve seeds at 160°C

[0031] 8.12gH 2 O and 0.092g aluminum sulfate are mixed uniformly, then add 0.38g NaOH, then add 3.32g silica sol under stirring, continue to stir until the solution becomes uniform, add ZSM-5 molecular sieve accounting for 10% of the mass of the silicon source as a seed crystal, and stir After uniformity, the gel was added into a polytetrafluoroethylene stainless steel reactor, and crystallized in an oven at 160°C for 8 hours. The product was filtered with suction and dried.

[0032] attached figure 2 The XRD spectrum of the ZSM-5 zeolite molecular sieve prepared by the seed crystal method shows that the product has a typical ZSM-5 zeolite molecular sieve structure, and the sample has a high degree of crystallinity.

Embodiment 3

[0033] Example 3: Crystallization of the universal precursor with the addition of MOR zeolite molecular sieve seeds at 160°C

[0034] 8.12gH 2 O and 0.092g of aluminum sulfate are mixed evenly, and then 0.38g of NaOH is added to it, and then 3.32g of silica sol is added under stirring, and the stirring is continued until the solution becomes uniform, and 10% of the mass of the silicon source is added as a MOR molecular sieve as a seed crystal, and after stirring , put the gel into a polytetrafluoroethylene stainless steel reactor, and crystallize it in an oven at 160°C for 12h. The product was filtered with suction and dried.

[0035] attached image 3 The XRD spectrum of the MOR zeolite molecular sieve prepared by the seed crystal method, it can be seen from the spectrum that the product has a typical MOR zeolite molecular sieve structure, and the sample has a high degree of crystallinity.

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Abstract

Relating to molecular sieve preparation methods, the invention aims to provide a method for synthesis of a high silicon zeolite molecular sieve with universal gel. The method includes the steps of: mixing deionized water with an aluminum source evenly, then adding NaOH, adding a silicon source under stirring, performing stirring continuously until the solution forms a silica-alumina gel; adding a zeolite molecular sieve seed crystal into the silica-alumina gel, performing stirring, then placing the mixture into a reaction kettle, and carrying out pumping filtration and drying on a crystallization product, thus obtaining raw powder of the high silicon zeolite molecular sieve. The product obtained by the invention not only maintains good crystallinity and purity, but also has good catalytic reaction activity. The whole production process does not use organic template agent, also greatly shortens the crystallization time through seed crystal synthesis, thus reducing unnecessary loss in the production process. The adopted inorganic raw materials are environment-friendly and low in price. Therefore, the method provided by the invention is of important significance for the basic research of zeolite molecular sieve and application in the field of actual chemical production.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for synthesizing a series of high-silica zeolite molecular sieves with universal gel. Background technique [0002] Zeolite molecular sieves are widely used in the fields of catalysis, ion exchange, adsorption and separation due to their open structure and large surface area. The initial zeolites (A, X, Y) were synthesized without organic templates. With the introduction of organic templates into the synthesis of zeolite molecular sieves, the types of zeolite molecular sieves have become rich and colorful. However, the use of these organic templates has many disadvantages: high synthesis cost, high toxicity, and serious waste liquid and gas emissions. In recent years, considering the disadvantages brought by the use of organic templates, synthesis without organic templates has been proposed again. Among them, the seed crystal synthesis is a new synthetic meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/38C01B39/42C01B39/44
CPCC01B39/02C01B39/38C01B39/42C01B39/44C01P2002/72
Inventor 孟祥举吴勤明朱龙凤肖丰收
Owner ZHEJIANG UNIV
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