Method for synthesizing high-crystallinity ZSM-5 molecular sieve without organic template

An organic template agent and high crystallinity technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of high energy consumption, achieve high single-pot yield, and be environmentally friendly , The effect of simple process

Inactive Publication Date: 2008-05-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this patented method is high energy consumption and the need to use inorganic acids that are corrosive to equipment

Method used

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  • Method for synthesizing high-crystallinity ZSM-5 molecular sieve without organic template
  • Method for synthesizing high-crystallinity ZSM-5 molecular sieve without organic template

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 0.480 gram of sodium hydroxide is dissolved in 28.69 gram of water, after stirring until clarification, add 0.796 gram of sodium aluminate (Al 2 o 3 41.0wt%, Na 2 O2 4.9wt%, H 2 (24.1 wt%) and 3.846 grams of solid silica gel (100-200 mesh), stirred for 1 hour to obtain a uniform gel. The gel was transferred to a 100mL polytetrafluoroethylene-lined stainless steel crystallization kettle, sealed and then crystallized with stirring at 190°C for 12 hours. After suction filtration, washing and drying, 6.72g of solid product was obtained.

[0027] The solid product was analyzed by X-ray diffraction to be ZSM-5 molecular sieve (see Figure 1), with a relative crystallinity of 102%.

[0028] In the present embodiment, the mol ratio between each component of reaction mixture is as follows:

[0029] SiO 2 :Al 2 o 3 =20:1, Na 2 O: SiO 2 =0.14:1, H 2 O: SiO 2 =25:1.

Embodiment 2

[0035] 5.457 grams of sodium silicate (SiO 2 21.15wt%, Na 2 O2 1.82wt%, H 2 (257.03wt%) was dissolved in 34.30 grams of water, and stirred until clarified to obtain solution A; in another beaker, 0.796 grams of sodium aluminate (Al 2 o 3 41.0wt%, Na 2 O2 4.9wt%, H 2(24.1wt%) was dissolved in 34.30 g of water, and stirred until clear to obtain solution B. Quickly add solution B to solution A at room temperature, then add 8.462 g of solid silica gel (100-200 mesh) while stirring, and continue stirring for 1 hour after the addition to obtain a uniform gel. The gel was transferred to a 100mL polytetrafluoroethylene-lined stainless steel crystallization kettle, sealed and then crystallized with stirring at 180°C for 72 hours. After suction filtration, washing, and drying, 5.44 g of a solid product was obtained.

[0036] The solid product was analyzed by X-ray diffraction to be ZSM-5 molecular sieve with a relative crystallinity of 114%.

[0037] In the present embodiment, th...

Embodiment 3

[0040] 4.608 gram of sodium hydroxide is dissolved in 71.46 gram of water, after stirring until clarification, add 1.592 gram of sodium aluminate (Al 2 o 3 41.0wt%, Na 2 O2 4.9wt%, H 2 (24.1 wt%) and 19.23 g of solid silica gel (100-200 mesh), stirred for 1 hour to obtain a uniform gel. The gel was transferred to a 100mL polytetrafluoroethylene-lined stainless steel crystallization kettle, sealed and then crystallized with stirring at 190°C for 24 hours. After suction filtration, washing and drying, 9.08g of solid product was obtained.

[0041] The solid product was analyzed by X-ray diffraction to be ZSM-5 molecular sieve with a relative crystallinity of 172%.

[0042] In the present embodiment, the mol ratio between each component of reaction mixture is as follows:

[0043] SiO 2 :Al 2 o 3 =50:1, Na 2 O: SiO 2 =0.2:1, H 2 O: SiO 2 =12.5:1.

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Abstract

The invention discloses a synthesizing method of high crystallinity ZSM-5 molecular sieve without using organic template, comprising the following steps: mixing silicon source and aluminum source with de-ionized water and inorganic base (needless if two silicon source is used) according to a certain proportion, wherein, the silicon source is unbodied solid of silicon dioxide or the mixture of the unbodied solid of silicon dioxide and solid metasilicate, and the aluminum source is aluminate or aluminum compounds; placing the mixture in a stainless steel reaction kettle provided with a teflon lining and performing hydrothermal crystallization under certain condition. The invention is characterized in that the high crystallinity ZSM-5 molecular sieve can be obtained without adding crystal seed into the mixture; and the ratio of water to silicon is small and the solid content is high; the expensive and environment-unfriendly organic template and the corrosive inorganic acid are not used. The invention has the advantages of low production cost, high productivity of single kettle, simple technology and environmental protection.

Description

technical field [0001] The invention belongs to a method for synthesizing zeolite molecular sieves, in particular to a method for synthesizing high-crystallinity ZSM-5 molecular sieves without an organic template. Background technique [0002] ZSM-5 molecular sieve is a high silica zeolite with a three-dimensional pore structure first developed by Mobil Corporation of the United States in the early 1970s (US3702886, 1972). Due to the unique structure of ZSM-5 molecular sieve, as well as good thermal stability and hydrothermal stability, it is suitable for alkylation, isomerization, disproportionation, type-selective reaction, catalytic cracking, methanol to gasoline, deep cracking of heavy oil, methanol Olefins and other reactions have unique catalytic properties, so they are widely used as catalyst materials and catalyst supports. [0003] The synthesis method of ZSM-5 molecular sieve can be generally divided into organic method and inorganic method. The so-called organic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 厉刚郑少烽方文军林瑞森
Owner ZHEJIANG UNIV
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