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Synthetic method for hierarchical-pore ZSM-5 molecular sieve

A technology of ZSM-5 and synthesis method, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high cost, heavy environmental pollution, and expensive carbon templates, and achieve high yield, The effect of reducing production costs

Active Publication Date: 2016-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the samples obtained by the above methods can be calcined at high temperature to obtain molecular sieves containing both mesoporous and microporous structures, the carbon templates used in the above methods are expensive, the synthesis operation process is complicated, and all involve the use of a large number of micropore directing agents. , so the cost is high, the environment is polluted heavily, and it is not suitable for large-scale industrial applications

Method used

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  • Synthetic method for hierarchical-pore ZSM-5 molecular sieve
  • Synthetic method for hierarchical-pore ZSM-5 molecular sieve
  • Synthetic method for hierarchical-pore ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Example 1 Sample 1 # preparation of

[0080] 0.10g of sodium metaaluminate was dissolved in 0.61 (25wt%) g of n-butylamine aqueous solution, and then 5.25g of silica sol (SiO 2 : 30.54wt%) was added dropwise into the solution obtained above, and continued to stir rapidly at room temperature for 2h until the mixture was uniform to obtain the initial gel mixture A. The molar ratio of each raw material in the initial gel mixture A is as follows: 50SiO 2 : 2.0NaAlO 2 : 3.9C 4 h 11 N: 427H 2 O. The initial gel mixture A was transferred to a PTFE-lined stainless steel reactor, and after dynamic crystallization at 160 °C for 5 h, it was cooled to room temperature to obtain precursor I.

[0081] Dissolve 0.62g of sodium metaaluminate and 0.40g of sodium hydroxide in 20g of deionized water, then gradually add 10.00g of white carbon black to the above-mentioned clear solution under rapid stirring (300rmp), and add 44.8g of Ionized water, continue to stir at room temperatu...

Embodiment 2

[0085] Example 2 Sample 2 # ~20 # preparation of

[0086] sample 2 # ~20 # The raw material type, raw material proportioning, crystallization condition are shown in Table 1, and batching process is the same as sample 1 in embodiment 1 # preparation.

[0087] Table 1 Molecular sieve synthesis ingredients and crystallization conditions

[0088]

[0089]

[0090] a : In the initial gel mixture A, the amount of silicon source added is SiO 2 The number of moles; the amount of aluminum source added in Al 2 o 3 The number of moles of template agent R is calculated by the number of moles of template agent R itself; the amount of water added is calculated by the number of moles of water itself.

[0091] b : In the initial gel mixture B, the addition amount of silicon source is SiO 2 The number of moles; the amount of aluminum source added in Al 2 o 3 The number of moles of the alkali source is calculated by the number of moles of the alkali source itself, if the alka...

Embodiment 3

[0098] Example 3 Sample 1 # ~20 # and comparative sample 1 # ~3 # XRD analysis

[0099] Sample 1 was analyzed by X-ray diffraction method # ~20 # and comparative sample 1 # ~3 # phase analysis.

[0100] The result shows that the sample 1 prepared by embodiment 1 and 2 # ~20 # and comparative sample 1 # ~3 # Both are high-purity and high-crystallinity ZSM-5 molecular sieves, typical representatives such as figure 1 Medium sample 1 # The XRD spectrum. sample 2 # ~20 # and comparative sample 1 # ~3 # The XRD spectrum result and figure 1 Close, that is, the position and shape of the diffraction peaks are basically the same, and the relative peak intensity fluctuates within ±5% according to the change of synthesis conditions, indicating that sample 1 # ~20 # and comparative sample 1 # ~3 # It has the characteristics of ZSM-5 structure and no miscellaneous crystals.

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Abstract

The invention relates to a synthetic method for a hierarchical-pore ZSM-5 molecular sieve. The method synthesizes the hierarchical-pore ZSM-5 molecular sieve with a high crystallization degree, strong acidity and good hydro-thermal stability from a small amount of a microporous template and a polymer of quaternary ammonium salt without usage of a hard template.

Description

technical field [0001] The application relates to a method for synthesizing a multi-stage porous ZSM-5 molecular sieve. The present application also relates to the application of the above-mentioned hierarchically porous ZSM-5 molecular sieve as a solid acid catalyst. Background technique [0002] Mobil Corporation of the United States first reported the synthesis of ZSM-5 molecular sieves in 1972. The material has become one of the most important molecular sieve catalytic materials in industrial applications due to its pore structure, adjustable acid center strength and density, high stability and unique shape-selective properties. [0003] However, due to the single pore structure and small pore size of ZSM-5 molecular sieve, the diffusion resistance of large-sized molecules in the pores is increased, which limits its application in catalytic reactions involving large molecules. In recent years, researchers have tried various methods to introduce mesopores into zeolites ...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J29/40
Inventor 王林英田鹏刘中民杨虹熠袁扬扬王德花
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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