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Preparation method of silicon-aluminum ZSM-22 molecular sieve with controllable grain size

A technology of crystal grain size and molecular sieve, applied in the directions of crystalline aluminosilicate zeolite, molecular sieve and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of complex synthesis steps, low product yield, etc. The effect of simplifying experimental steps and improving utilization

Pending Publication Date: 2021-07-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN109502607A discloses a method for synthesizing molecular sieves with a particle size of less than 100nm. Pre-crystallization is used to obtain the initial aluminosilicate mixture and the secondary hydrothermal crystallization of the mixture. The synthesis steps are relatively complicated and the product yield is low

Method used

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  • Preparation method of silicon-aluminum ZSM-22 molecular sieve with controllable grain size
  • Preparation method of silicon-aluminum ZSM-22 molecular sieve with controllable grain size
  • Preparation method of silicon-aluminum ZSM-22 molecular sieve with controllable grain size

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] First, silica sol, Al 2 SO 4 , 1,6-hexanediamine, potassium hydroxide, and deionized water are mixed according to the following molar ratio to form an initial gel mixture, silica sol (as SiO 2 Count): Al 2 SO 4 (in Al 2 o 3 Total): 1,6-Hexamethylenediamine: Potassium Hydroxide: Deionized Water = 1:0.0125:0.1:0.2:30. The obtained mixture was placed in a reaction kettle lined with polytetrafluoroethylene, and after dynamic crystallization at a speed of 40 rpm at 150 ° C for 10 h, it was taken out and cooled, and KOH, K + / SiO 2 The molar ratio is 0.02:1. After stirring for 2 hours, secondary crystallization at 150°C at 40 rpm for 24 hours under autogenous pressure. After the crystallization is complete, the product is filtered and washed until neutral, dried and calcined to obtain a silica-alumina molecular sieve. Wherein, the calcination temperature is 600° C., and the calcination time is 10 h.

[0039] Its structure is ZSM-22 zeolite molecular sieve by X-ray di...

Embodiment 2

[0042] First, silica sol, Al 2 SO 4, 1,6-hexanediamine, potassium hydroxide, and deionized water are mixed according to the following molar ratio to form an initial gel mixture, silica sol (as SiO 2 Count): Al 2 SO 4 (in Al 2 o 3 Total): 1,6-Hexamethylenediamine: Potassium Hydroxide: Deionized Water = 1:0.0125:0.2:0.2:30. The obtained mixture was placed in a reaction kettle lined with polytetrafluoroethylene, and after dynamic crystallization at a speed of 40 rpm at 160°C for 12 hours, it was taken out and cooled, and HNO was added 3 solution, H + / SiO 2 The molar ratio is 0.02:1. After stirring for 2 hours, secondary crystallization was performed at 160°C at 40 rpm for 24 hours under autogenous pressure. After the crystallization was completed, the product was filtered and washed until neutral, dried and calcined to obtain a silica-alumina molecular sieve. Wherein, the calcination temperature is 600° C., and the calcination time is 10 h.

[0043] Its structure is ZS...

Embodiment 3

[0046] First, silica sol, Al 2 SO 4 , 1,6-hexanediamine, potassium hydroxide, and deionized water are mixed according to the following molar ratio to form an initial gel mixture, silica sol (as SiO 2 Count): Al 2 SO 4 (in Al 2 o 3 Total): 1,6-Hexamethylenediamine: Potassium Hydroxide: Deionized Water = 1:0.015:0.2:0.2:40. The obtained mixture was placed in a reaction kettle lined with polytetrafluoroethylene, and after dynamic crystallization at a speed of 40 rpm at 160 °C for 10 h under autogenous pressure, it was taken out and cooled, and H 2 SO 4 solution, H + / SiO 2 The molar ratio is 0.06:1. After stirring for 2 hours, the secondary crystallization is carried out at 160°C at a speed of 40 rpm for 28 hours under autogenous pressure. After the crystallization is completed, the product is filtered and washed until neutral, dried and calcined to obtain a silica-alumina molecular sieve. Wherein, the calcination temperature is 500° C., and the calcination time is 8 ho...

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Abstract

The invention relates to the technical field of preparation of inorganic porous materials, in particular to a preparation method of a silicon-aluminum ZSM-22 molecular sieve with a controllable grain size, which comprises the following steps of adding a silicon source, an aluminum source, an alkali source, a template agent and deionized water as reaction raw materials, carrying out crystallization reaction in a hydrothermal system, directly taking out after a certain time, adding an additive, and carrying out secondary crystallization reaction. According to the method, controllable synthesis of the molecular sieve in a certain range can be realized by adjusting the variety and dosage of the additives, the synthesis steps are simple, and the product yield is greatly improved. When the small-grain silicon-aluminum ZSM-22 molecular sieve is applied to a Fischer-Tropsch synthesis product isomerization reaction, the isomerization activity can be obviously improved, and the small-grain silicon-aluminum ZSM-22 molecular sieve has a relatively good industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic porous materials, in particular to a preparation method of silicon-aluminum ZSM-22 molecular sieve with controllable grain size. [0002] technical background [0003] Si-alumina ZSM-22 molecular sieve is a microporous, high-silica molecular sieve developed by Mobil Corporation of the United States in the 1980s. Its skeleton includes five-membered ring, six-membered ring and ten-membered ring structure, belongs to the TON topology, has only one-dimensional ten-membered ring channels, no intersecting channels, and its channel size is 4.5 Å×5.5 Å. The suitable pore structure and strong acidity of ZSM-22 are used in the isomerization reaction of n-paraffins, showing good activity, selectivity and stability. [0004] The particle size and morphology of molecular sieves are important factors affecting the catalytic performance of molecular sieves. The synthesis and preparation of sili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/04B82Y30/00B82Y40/00
CPCC01B39/48C01B39/04B82Y30/00B82Y40/00C01P2004/64C01P2006/80C01P2004/03C01P2004/62
Inventor 李德宝王乐侯博郗宏娟牛鹏宇贾丽涛马中义陈从标
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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