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Method for preparing ZSM-5 zeolite by in situ crystallization

An in-situ crystallization, ZSM-5 technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminum silicate zeolite, etc., can solve the problem of small micropore area and micropore volume , Complicated methods, low ZSM-5 zeolite content, etc., to achieve the effect of rich mesopores, increased micropore volume, and high zeolite content

Active Publication Date: 2009-06-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of preparing ZSM-5 zeolite by this method is relatively complicated, and the crystallization time is as long as 72 hours, and the content of ZSM-5 zeolite in the crystallized microspheres is low, and the micropore area and micropore volume are small

Method used

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  • Method for preparing ZSM-5 zeolite by in situ crystallization
  • Method for preparing ZSM-5 zeolite by in situ crystallization
  • Method for preparing ZSM-5 zeolite by in situ crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Preparation of microspheres

[0039] Add kaolin, diatomite, bentonite, silica sol and water into a gel tank and mix homogeneously so that the solid content of the slurry is 30% by weight. The slurry is spray-dried to obtain microspheres with an average particle diameter of 50 μm. The microspheres were washed twice with decationized water of pH=2-4 at a mass ratio of 10:1 to the microspheres. The properties of raw materials are shown in Table 1, and the composition content of each component in the slurry is calculated on a dry basis in Table 2.

[0040] Table 1

[0041]

[0042] Table 2

[0043] Composition (dry basis, parts by weight, adhesive is SiO 2 count) Example 1 Kaolin 5, diatomaceous earth 35, bentonite 45, silica sol 15 Example 2 Kaolin 45, diatomaceous earth 35, water glass 20 Example 3 Kaolin 20, pyrophyllite 60, silica sol 20 Example 4 Kaolin 70, diatomaceous earth 1, ZSM-5 zeolite variety 5, silica sol 24 ...

Embodiment 2

[0049] 1. Preparation of microspheres

[0050] Microspheres were prepared according to the method for preparing microspheres described in Example 1, except that the slurry was prepared according to the formula in Example 2 in Table 2.

[0051] 2. Calcination of microspheres and in situ hydrothermal crystallization

[0052] The obtained microspheres were calcined at a temperature of 800° C. for 3 hours to obtain calcined microspheres, and the active SiO2 in the calcined microspheres 2 The content is 65% by weight.

[0053] Get the microsphere after 23.8g roasting, mix with 1.42g sodium hydroxide and 67.5g water, wherein the active SiO in the microsphere 2 with OH - The molar ratio is 1:0.14. The mixture was moved into a stainless steel kettle with a polytetrafluoroethylene liner, and was subjected to static constant temperature crystallization at a temperature of 170° C. for 12 hours, and then the solid product was separated, filtered with suction, washed and dried to obtai...

Embodiment 3

[0056] 1. Preparation of microspheres

[0057] Microspheres were prepared according to the method for preparing microspheres described in Example 1, except that the slurry was prepared according to the formula in Example 3 in Table 2.

[0058] 2. Calcination of microspheres and in situ hydrothermal crystallization

[0059] The obtained microspheres were calcined at a temperature of 700° C. for 4 hours to obtain calcined microspheres, and the active SiO2 in the calcined microspheres 2 The content is 53% by weight.

[0060] Get 14.3g calcined microspheres, mix with 1.95g sodium hydroxide, 3.51g n-butylamine and 108g water, wherein the active SiO in the microspheres 2 with OH - The molar ratio is 1:0.39, the active SiO 2 The molar ratio with n-butylamine is 1:0.38. Move the mixture into a stainless steel kettle with a polytetrafluoroethylene liner, raise the temperature from room temperature to 110°C within 1 hour, dynamically crystallize at a temperature of 110°C for 20 hou...

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Abstract

The invention relates to a method for preparing ZSM-5 zeolite through in-situ crystallization, which comprises that: slurry containing kaolin and water is prepared into microspheres through spray drying; the prepared microspheres are baked; and the baked microspheres are mixed with a water solution containing alkali, and the mixture is subjected to in-situ hydrothermal crystallization to obtain crystallization product, wherein the slurry also contains silicon-enriched clay, and the mol ratio of SiO2 to Al2O3 in the silicon-enriched clay is more than 2. The ZSM-5 zeolite prepared by the method has high content of zeolite and rich middle holes, so the ZSM-5 zeolite can be used as a catalyst in the field of petrochemical industry, in particular as a catalytic agent in the FCC process to improve propylene yield.

Description

technical field [0001] The invention relates to a method for preparing ZSM-5 zeolite by in-situ crystallization. Background technique [0002] Since ZSM-5 zeolite was first reported by the Mobil Company of the United States (USP3702886) in 1972, due to the unique three-dimensional pore structure and shape-selective catalysis of ZSM-5 zeolite, it has high silicon-aluminum ratio and lipophilic and hydrophobic characteristics. Characterized by high stability and high catalytic activity, it is widely used as a catalyst or catalytic assistant in various methods. [0003] ZSM-5 zeolites have been shown to be particularly useful catalysts in reactions involving aromatic compounds, especially aromatic compounds having a single carbocyclic ring. Therefore, in the conversion reaction of olefins, naphthalene, alcohols, ethers and alkanes to aromatic compounds and in reactions such as isomerization, alkylation, dealkylation and transalkylation of aromatic compounds, ZSM-5 zeolite All ...

Claims

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Application Information

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IPC IPC(8): C01B39/38C01B39/40B01J29/40
Inventor 潘晖华罗一斌王殿中慕旭宏蒋文斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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