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Method for synthesizing ZSM-5 zeolite

A technology of ZSM-5 and zeolite, which is applied in the field of synthesizing ZSM-5 zeolite, can solve the problems of difficult operation and long cooling time, and achieve the effects of high single-pot yield, short crystallization time and low operating cost

Active Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a single silica sol as the silicon source. It is easy to heat up in actual operation, but it takes a long time to cool down. Therefore, it is difficult to operate at high temperature first and then at low temperature.

Method used

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  • Method for synthesizing ZSM-5 zeolite
  • Method for synthesizing ZSM-5 zeolite
  • Method for synthesizing ZSM-5 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 200 grams of water glass, add 442 grams of water and 76.5 grams of low bias to it, stir for 30 minutes, add 133 grams of silica gel and 35.5 grams of NaY zeolite, and stir for 30 minutes to obtain a uniform gel. The gel was transferred to a 2-liter stainless steel crystallization kettle, sealed, and then dynamically crystallized at 170° C. for 14 hours at a stirring speed of 100 rpm. The solid product was obtained after suction filtration, washing, and drying. The solid product was analyzed by X-ray diffraction to be a pure phase ZSM-5 zeolite with a relative crystallinity of 103%. In the present embodiment, the mol ratio between each component of reaction mixture is as follows: Na 2 O / SiO 2 =0.13:1, SiO 2 / Al 2 o 3 =25:1,H 2 O / SiO 2 =12. Seed / SiO 2 (weight ratio) = 0.15:1. Among them, the active silicon source accounts for 24% of the total silicon source. The particle size distribution of the obtained ZSM-5 zeolite is shown in Table 2.

Embodiment 2

[0028] Take 372 grams of water glass, add 396 grams of water and 178 grams of low bias to it, stir for 30 minutes, add 282 grams of silica gel and 17 grams of ZSM-5 zeolite, and stir for 30 minutes to obtain a uniform gel. The gel was transferred to a 2-liter stainless steel crystallization kettle, sealed, and dynamically crystallized at 180° C. for 12 hours at a dynamic crystallization stirring speed of 100 rpm. After suction filtration, washing, and drying, a solid product was obtained. The solid product was analyzed by X-ray diffraction to be a pure phase ZSM-5 zeolite with a relative crystallinity of 105%. In the present embodiment, the mol ratio between each component of reaction mixture is as follows: Na 2 O / SiO 2 =0.15:1, SiO 2 / Al 2 o 3 =40:1,H 2 O / SiO 2 =8. Seed / SiO 2 (weight ratio) = 0.05:1. Among them, the active silicon source accounts for 22% of the total silicon source.

Embodiment 3

[0030]Take 255 grams of silica sol A, add 417 grams of water and 11.7 grams of NaOH to it, stir for 30 minutes, add 45 grams of low bias, stir for 30 minutes, add 133 grams of silica gel and 20.7 grams of NaY zeolite, and stir for 30 minutes to obtain a uniform gel . The gel was transferred to a 2-liter stainless steel crystallization kettle, sealed and dynamically crystallized at 160° C. for 16 hours at a rotation speed of 100 rpm. The solid product was obtained after suction filtration, washing and drying. After the crystallization was completed, solid-liquid separation collected 360 grams of mother liquor (SiO in mother liquor 2 The content is 4.68% by weight, Na 2 The O content is 1.30% by weight). The collected solid product was analyzed by X-ray diffraction to be a pure phase ZSM-5 zeolite with a relative crystallinity of 100%. In the present embodiment, the molar ratio between each component of reaction mixture is as follows: Na 2 O / SiO 2 =0.07:1, SiO 2 / Al 2 o ...

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Abstract

The invention discloses a method for synthesizing zeolite Socony Mobil (ZSM)-5 zeolite. The method comprises the following steps of: mixing a composite silicon source, an aluminum source and water, adding or not adding inorganic alkali, and crystallizing an obtained reaction mixture at the temperature of between 100 and 200 DEG C for 8 to 16 hours, wherein in the reaction mixture, the molar ratio of Na2O to SiO2 is 0.05-0.2:1, the molar ratio of SiO2 to Al2O3 is 20-100:1 and the molar ratio of H2O to SiO2 is 5-15:1, and the composite silicon source consists of an active silicon source in an amount which is 13 to 99 weight percent based on the SiO2 and an inert silicon source in an amount which is 1 to 87 weight percent based on the SiO2. The method for synthesizing the ZSM-5 zeolite has low water consumption, high yield in a single kettle, short crystallization time and low cost; and the synthesized ZSM-5 zeolite has high crystallinity and uniform particle size.

Description

technical field [0001] The invention relates to a method for synthesizing ZSM-5 zeolite. Background technique [0002] ZSM-5 zeolite was first reported by Mobil Corporation of the United States in 1972 (USP3702886), because of its high silicon-aluminum ratio, good thermal and hydrothermal stability, lipophilic and hydrophobic characteristics, and unique three-dimensional pore structure and shape-selective catalysis It has unique catalytic properties for reactions such as alkylation, isomerization, disproportionation, shape-selective reaction, catalytic cracking, methanol-to-gasoline, and methanol-to-olefins, and is widely used in the petrochemical field. [0003] The synthesis method of ZSM-5 zeolite can be divided into organic method and inorganic method. The so-called organic method is to use an organic template in the reaction system, and the inorganic method is to use no organic template in the reaction system. Organic templates are expensive and pollute the environmen...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 潘晖华罗一斌王殿中舒兴田何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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