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Method for synthesizing ZSM-5 zeolite

A ZSM-5, synthesis method technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of discharge of sodium sulfate-containing waste liquid, pollution of the environment, waste of resources, etc. , to achieve the effect of high yield per reactor, environmental protection and zero emission

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

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Problems solved by technology

[0007] In the existing method of synthesizing ZSM-5 without template, a large amount of synthetic mother liquor containing silicon and sodium is produced. The direct discharge of this mother liquor not only pollutes the environment, but also causes waste of resources. Usually sulfuric acid or aluminum sulfate is used to precipitate silicon in the mother liquor, but There will be discharge problems of waste liquid containing sodium sulfate

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

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Embodiment 1

[0022] To the volume of 1m 3 Add 60 kg of deionized water, 5.1 kg of low bias, 10 kg of 20% by weight NaOH solution, 24.6 kg of coarse-pore silica gel and 2.4 kg of NaY zeolite in the crystallization kettle, and stir for 30 minutes to obtain a uniform gel. Dynamic crystallization was carried out at 180° C. for 17 hours, and the stirring speed of dynamic crystallization was 15 rpm. Then cool to room temperature and filter to obtain mother liquor and filter cake. The filter cake is washed and dried to obtain a solid product. The solid product is analyzed by X-ray diffraction to be a pure phase ZSM-5 zeolite with a relative crystallinity of 100%. In the present embodiment, the mol ratio between each component of reaction mixture is as follows: Na 2 O / SiO 2 =0.1:1, SiO 2 / Al 2 o 3 =50:1, H 2 O / SiO 2 =10:1. Seed / SiO 2 (weight ratio) = 0.08:1. Obtain 41 kilograms of mother liquor, SiO in mother liquor 2 The content is 5.97% by weight, Na 2 The O content is 2.20% by weig...

Embodiment 2

[0024] to 1m 3 Add 26 kilograms of deionized water, 41 kilograms of the mother liquor obtained in Example 1, 5.1 kilograms of low bias, 5.2 kilograms of 20% by weight NaOH solution, 21.9 kilograms of coarse-pore silica gel and 2.4 kilograms of NaY in the crystallization kettle, and stir for 30 minutes. A uniform gel was obtained, sealed, and dynamically crystallized at 180° C. for 12 hours, and the stirring speed of dynamic crystallization was 15 rpm. Then cool to room temperature, filter to obtain the mother liquor and filter cake, and the filter cake is washed and dried to obtain a solid product. The solid product was analyzed by X-ray diffraction to be a pure phase ZSM-5 zeolite with a relative crystallinity of 102%. In the present embodiment, the mol ratio between each component of reaction mixture is as follows: Na 2 O / SiO 2 =0.1:1, SiO 2 / Al 2 o 3 =50:1, H 2 O / SiO 2 =10:1. Seed / SiO 2 (weight ratio) = 0.08:1. Obtain 41 kilograms of mother liquor, SiO in mother ...

Embodiment 3

[0026] With embodiment 2, difference is to add the mother liquor that 41 kilograms of embodiment 2 obtains. In this example, the solid product is a pure-phase ZSM-5 zeolite with a relative crystallinity of 102%. The molar ratio between the components of the reaction mixture is as follows: Na 2 O / SiO 2 =0.1:1, SiO 2 / Al 2 o 3 =50:1, H 2 O / SiO 2 =10:1. Seed / SiO 2 (weight ratio) = 0.08:1. Obtain 41 kilograms of mother liquor, SiO in mother liquor 2 The content is 5.96% by weight, Na 2 The O content was 2.22% by weight.

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Abstract

The invention discloses a method for synthesizing ZSM-5 zeolite. The method comprises the following steps of: mixing an amorphous silicon dioxide solid silicon source, an aluminate aluminium source, water and ZSM-5 synthesizing mother liquor, crystallizing the mixture at the temperature of between 110 and 200 DEG C for 8 to 24 hours; and filtering, washing and drying the crystallized mixture to obtain ZSM-5 zeolite, wherein molar ratios of the components in the mixture are that: M2O / SiO2 is equal to 0.05-0.2:1, SiO2 / Al2O3 is equal to 20-100:1, and H2O / SiO2 is equal to 5-15:1; and M is an alkali metal. In the method for synthesizing the ZSM-5 zeolite, the process is simple; the yield of single kettle is high; the crystallizing time is short; the emission of the mother liquor is reduced or zero emission of the mother liquor is realized; the synthesis and operation cost is relatively low; the B acid content of the obtained ZSM-5 zeolite is high; and the L acid content of the obtained ZSM-5 zeolite is low.

Description

technical field [0001] The invention relates to a ZSM-5 zeolite and a synthesis method thereof. Background technique [0002] ZSM-5 has high silicon-aluminum ratio, good thermal and hydrothermal stability, lipophilic and hydrophobic characteristics, three-dimensional pore structure and shape-selective catalysis. Cracking, methanol to gasoline, methanol to olefins and other reactions have unique catalytic properties and are widely used in petrochemical fields. [0003] ZSM-5 zeolite was first reported by Mobil Corporation of the United States in 1972 (USP3702886), and its synthesis method can generally 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. The organic template is expensive and pollutes the environment, and the ZSM-5 zeolite synthesized by using the organic template needs to be calcined at high temper...

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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