Method for solid-phase synthesis of ZSM-5 molecular sieve by using silica fume

A ZSM-5, solid-phase synthesis technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of large resource utilization of micro-silica powder, high production efficiency, single Problems such as high pot yield

Inactive Publication Date: 2016-10-12
YUNNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] 1. In view of the insufficient technology of existing synthetic ZSM-5 molecular sieves and the problem that the output of microsilica powder is very large and the utilization rate of resources is extremely low, one of the purposes of the present invention is to provide a method for directly using microsilica powder for solid-phase synthesis of ZSM -5 molecular sieve method, the method has low synthesis cost, simple treatment process, short crystallization time, fast reaction speed; high single-pot yield and high production efficiency; and the prepared ZSM-5 molecular sieve has high crystallinity, physical and chemical excellent performance

Method used

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  • Method for solid-phase synthesis of ZSM-5 molecular sieve by using silica fume
  • Method for solid-phase synthesis of ZSM-5 molecular sieve by using silica fume
  • Method for solid-phase synthesis of ZSM-5 molecular sieve by using silica fume

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Weigh 1.315g of sodium silicate, 0.43g of ammonium chloride, 0.24g of TPABr, 0.33g of microsilica, pour it into a mortar, grind and mix for 20 minutes, put the mixture into a PTFE-lined steel reaction vessel In the kettle, crystallize at 130°C for 48h, after cooling, the reactant is ground, dissolved, suction filtered and dried in a blast drying oven at 60°C for 12 hours to obtain the final product. attached figure 1 From the characterization results of the product's XRD, it can be seen that the product has a typical MFI structure with good crystallinity. figure 2 It is a scanning electron microscope photograph of the product of Example 1.

Embodiment 2

[0029] Weigh 1.315g of sodium silicate, 0.43g of ammonium chloride, 0.24g of TPABr, and 0.33g of microsilica powder, pour it into a mortar, grind and mix for 20 minutes, then put the mixture into a Teflon-lined steel reaction vessel. In the kettle, crystallize at 140°C for 36 hours, and after cooling, the reactants are ground, dissolved, suction filtered and dried in a blast drying oven at 60°C for 12 hours to obtain the final product. attached image 3 From the characterization results of the product's XRD, it can be seen that the product has a typical MFI structure with good crystallinity. Figure 4 It is a scanning electron microscope photograph of the product of Example 2.

Embodiment 3

[0031] Weigh 1.315g of sodium silicate, 0.43g of ammonium chloride, 0.24g of TPABr, and 0.33g of microsilica powder, pour it into a mortar, grind and mix for 20 minutes, then put the mixture into a Teflon-lined steel reaction vessel. In the kettle, crystallize at 160°C for 24h, after cooling, the reactants are ground, dissolved, suction filtered and dried in a blast drying oven at 60°C for 12 hours to obtain the final product. attached Figure 5 From the characterization results of the product's XRD, it can be seen that the product has a typical MFI structure with good crystallinity. Image 6 It is a scanning electron microscope photograph of the product of Example 3.

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Abstract

The invention discloses a method for synthesizing ZSM-5 molecular sieve in solid phase by using lignite, which belongs to the technical field of molecular sieve preparation; the invention uses industrial waste micro-silica powder, without any pretreatment, and directly mixes it with sodium silicate, template agent and alkali Sources were ground and mixed, and crystallized at 130-220°C for 1-48 hours. The reaction product was ground, dissolved, filtered, and dried to obtain ZSM-5 molecular sieve. The present invention uses micro-silicon powder that does not require any pretreatment as a silicon-aluminum source to replace Si and Al pure chemical reagents to synthesize molecular sieves, which not only reduces the synthesis cost of ZSM-5 molecular sieves, but also reduces environmental dust pollution caused by micro-silicon powder , It also realizes the high-value utilization of micro-silica fume. At the same time, the synthesis route only involves the mixing of initial raw materials without using any solvent, which avoids the waste caused by the use of a large amount of clean water resources and the pollution caused by a large amount of waste liquid containing organic plates. The synthesis process is simple, energy saving and emission reduction, There are huge industrial application prospects.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a kind of micro-silica powder using industrial waste, without any pretreatment, directly grinding and mixing with sodium silicate, template agent and alkali source, and crystallization reaction at 130-220° C. 1~48h, the reaction product is ground, dissolved, filtered and dried to obtain the method of ZSM-5 molecular sieve. Background technique [0002] Molecular sieves are crystalline aluminosilicates with uniform pore structure. Molecular sieves are widely used as industrial catalysts or catalyst carriers due to their well-defined pore distribution, extremely high specific surface area, and good thermal stability. With the increasing importance of molecular sieve catalysts in the industry, new types of molecular sieves have been greatly activated, ranging from molecular sieves with low and medium silicon ratios, to new molecular sieves with high silicon thre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2006/90
Inventor 陈秀华雷正涛朱文杰
Owner YUNNAN UNIV
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