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Method of preparing ZSM-5 molecular sieves

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., to achieve high synthesis yield, reduce production costs, and reduce the effect of viscosity

Active Publication Date: 2009-10-21
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the patent has been working hard to improve the efficiency of single-pot synthesis and reduce the amount of organic templates, templates still need to be used, and the patented method is used to synthesize molecular sieves with a high silicon-aluminum ratio (silicon-aluminum ratio greater than 100)

Method used

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  • Method of preparing ZSM-5 molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In a water bath at 60°C, the commercially available SiO 2 Content is 96.3wt% coarse porous silica gel 32.16g, water glass (containing SiO 2 27.25wt%, Na 2 O 8.75wt%) 202.17g and distilled water 107.32g, mixed and stirred for about 1 hour, then added aluminum sulfate solution, the aluminum sulfate solution is made with Al 2 o 3 15.1wt% Al 2 (SO 4 ) 3 18H 2 O 26.92g was obtained by adding 134.83g of distilled water. After stirring well, add 3M H 2 SO 4 Solution 40g, ZSM-5 seed crystal (synthesized in this laboratory, silicon-aluminum ratio 36) 10g, stirred for 40 minutes to prepare the mixture gel. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =36;Na 2 O / SiO 2 =0.12;H 2 O / SiO 2 =16. After sealing, heat up to 180°C and crystallize at a constant temperature for 24 hours under stirring. After the crystallization is completed, cool and filter to remove the mother liquor, wash and dry the filter cake to obtain a crys...

Embodiment 2

[0046] Under a water bath at 60°C, 39.94 g of coarse-porous silica gel, 203.47 g of water glass, and 101.34 g of distilled water were sequentially mixed together and stirred for 1 hour. Then add aluminum sulfate solution, the aluminum sulfate solution is made with Al 2 o 3 15.1wt% Al 2 (SO 4 ) 3 18H 2 O 23.53g was added to 141.73g of distilled water. After stirring well, add 3M H 2 SO 4 20 g of the solution, 10 g of ZSM-5 seed crystals (synthesized in our laboratory, with a silicon-aluminum ratio of 36), were stirred for 40 minutes to form a mixture gel. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 = 45; Na 2 O / SiO 2 =0.15;H 2 O / SiO 2 =14. After sealing, heat up to 180°C and crystallize at a constant temperature for 24 hours under stirring. After the crystallization is completed, cool and filter to remove the mother liquor, wash and dry the filter cake to obtain a crystallized product.

[0047] According to X-ray diff...

Embodiment 3

[0050] At room temperature, 132.18 g of coarse-porous silica gel, 140.03 g of distilled water, and 154.45 g of 20 wt % NaOH solution were mixed together and stirred for 1 hour. Then add aluminum sulfate solution, the aluminum sulfate solution is made with Al 2 o 3 15.1wt% Al 2 (SO 4 ) 3 18H 2 O 40.04g was added into 114.41g of distilled water to dissolve the obtained. Then add 15g of ZSM-5 seed crystals (synthesized in our laboratory, with a silicon-aluminum ratio of 36), and stir for 40 minutes to form a mixture gel. The molar ratio of each component in the gel according to its oxide is: SiO 2 / Al 2 o 3 =36;Na 2 O / SiO 2 =0.18;H 2 O / SiO 2 =10. After sealing, heat up to 180°C and crystallize at a constant temperature for 24 hours under stirring. After the crystallization is completed, cool and filter to remove the mother liquor, wash and dry the filter cake to obtain a crystallized product.

[0051] According to X-ray diffraction (XRD), its phase belongs to ZSM-5...

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Abstract

The invention provides a method of preparing ZSM-5 molecular sieves, which is favorable to the yield increase of the ZSM-5 molecular sieves. The method comprises the steps: using solid silica gel as all or partial silica sources, preparing the solid silica gel and water into reaction mixture gel at certain temperature and alkalinity, and carrying out hydrothermal crystallization of the reaction mixture gel by a conventional method in the presence of seed crystals. The molar ratio of components of the reaction mixture gel conforms to the following formula: 3-15 Na2O: 1Al2O3: 20-100SiO2: 100-1200 H2O. The invention can greatly improve the yield of synthesized ZSM-5 molecular sieves.

Description

technical field [0001] The invention belongs to molecular sieve and its preparation technology. Specifically, it relates to a method for preparing ZSM-5 molecular sieve by using solid silica gel as all or part of the silicon source. Background technique [0002] Since ZSM-5 zeolite molecular sieve was first reported by Mobil Corporation of the United States in 1972, organic amines have been considered as essential raw materials for the synthesis of ZSM-5 molecular sieve for a long time. In recent years, due to the high price and high toxicity of organic amines to synthesize ZSM-5 molecular sieves, in order to get rid of the dependence on organic amine templates, many scholars have begun to conduct extensive research and exploration on the synthesis of ZSM-5 molecular sieves from inorganic amines. . After the 1980s, the technology of using ZSM-5 molecular sieve seeds to synthesize ZSM-5 molecular sieves appeared, which significantly reduced the preparation cost of ZSM-5 mol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 申宝剑李金芝郝坤国玲玲孙兵
Owner BC P INC CHINA NAT PETROLEUM CORP
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