Hierarchical pore SAPO-34 molecular sieve synthesis method

A synthesis method and molecular sieve technology are applied in the directions of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of increased cost, cumbersome synthesis steps, unfavorable industrialized production, etc., and can improve the service life and reduce the cost of raw materials. Effect

Inactive Publication Date: 2018-02-16
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesis of multi-stage porous SAPO-34 molecular sieves requires acid or alkali post-treatment of SAPO-34 molecular sieves in the current research, or the introduction of other components into the mother liquor, which makes the synthesis steps cumbersome and costly, which is not conducive to large-scale Industrial production

Method used

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  • Hierarchical pore SAPO-34 molecular sieve synthesis method
  • Hierarchical pore SAPO-34 molecular sieve synthesis method
  • Hierarchical pore SAPO-34 molecular sieve synthesis method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] At room temperature, add water, water glass, aluminum isopropoxide, phosphoric acid and triethylamine to the beaker in turn, stir and mix thoroughly to obtain the initial gel mixture of SAPO-34 molecular sieve, the molar ratio of each component of the mixture is : 1.0Al 2 o 3 : 0.1 SiO 2 : 0.8P 2 o 5 : 1.5 Triethylamine: 10H 2 O. After the stirring, put the above-mentioned gel mixture into a stainless steel reactor, then put the reactor into a dynamic oven, raise the temperature to 160°C, and crystallize at a constant temperature for 60 hours. After the crystallization is completed, filter, wash, and dry to obtain a solid product, that is, the original powder of SAPO-34 molecular sieve. The original SAPO-34 molecular sieve powder was calcined in air at 650°C for 2 hours to remove the template agent contained in the original powder, and a white SAPO-34 molecular sieve with hierarchical pores was obtained. XRD spectrum as figure 1 As shown, the SEM photos are as ...

Embodiment 2

[0037] At room temperature, add water, sodium silicate, aluminum sol, ammonium phosphate and diethylamine to the beaker in turn, stir to make it fully mixed, and obtain the SAPO-34 molecular sieve initial gel mixture, and the molar ratio of each component of the mixture is : 1.0Al 2 o 3 : 0.6SiO2 2 : 1.2P 2 o 5 : 2.5 diethylamine: 50H 2 O. After the stirring, put the above gel mixture into a stainless steel reactor, then put the reactor into a dynamic oven, raise the temperature to 180°C, and crystallize at constant temperature for 8 hours. After the crystallization is completed, filter, wash, and dry to obtain a solid product, that is, the original powder of SAPO-34 molecular sieve. The original SAPO-34 molecular sieve powder was calcined in air at 500° C. for 10 h to remove the template agent contained in the original powder, and a white SAPO-34 molecular sieve with hierarchical pores was obtained. XRD spectrum as figure 1 As shown, the SEM photos are as image 3 sho...

Embodiment 3

[0039] At room temperature, add water, silica sol, pseudo-boehmite, phosphoric acid and triethylamine to the beaker in turn, stir and mix thoroughly to obtain the SAPO-34 molecular sieve initial gel mixture. The molar ratio of each component of the mixture is For: 1.0Al 2 o 3 : 0.44SiO2 2 : 1.1P 2 o 5 : 2.25 Triethylamine: 36H 2O. After the stirring, put the above gel mixture into a stainless steel reaction kettle, then put the reaction kettle into a dynamic oven, raise the temperature to 165° C., and crystallize at a constant temperature for 33 hours. After the crystallization is completed, filter, wash, and dry to obtain a solid product, that is, the original powder of SAPO-34 molecular sieve. The original SAPO-34 molecular sieve powder was calcined in air at 600°C for 6 hours to remove the template agent contained in the original powder, and a white SAPO-34 molecular sieve with hierarchical pores was obtained. XRD spectrum as figure 1 As shown, the SEM photos are as ...

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Abstract

The invention provides a hierarchical pore SAPO-34 molecular sieve synthesis method which is characterized in that an aluminum source, a silicon source, a phosphorus source, an organic template agentand water are mixed and added into a hydrothermal reactor, and in-situ synthesis is performed to form an SAPO-34 molecular sieve with hierarchical pores. According to the hierarchical pore SAPO-34 molecular sieve synthesis method, a hierarchical pore structure can be formed without acid or alkali post-treatment process or addition of other components, raw material cost and subsequent separation steps are reduced, industrial amplifying production is facilitated, substance diffusion and heat conduction in methanol-to-olefin reaction are facilitated by formation of the hierarchical pores, and theservice life of the molecular sieve is greatly prolonged.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, in particular to a method for synthesizing multi-level porous SAPO-34 molecular sieves. Background technique [0002] SAPO-34 molecular sieve (containing Si, Al, P and O elements) was first invented in 1984 by scientists from United Carbon Corporation (UCC). SAPO-34 molecular sieve is a kind of crystalline silicoaluminophosphate. Its molecular sieve framework is a three-dimensional framework structure composed of PO4, AlO4 and SiO4 tetrahedrons connected to each other. 0.65nm) and a three-dimensional pore structure, the effective diameter of the molecular sieve aperture is maintained between 0.43 and 0.50nm. Only small molecules below C3 and normal hydrocarbons can enter and exit the pores, and isohydrocarbons and aromatics are severely restricted. This property makes SAPO-34 molecular sieve have excellent shape selectivity, and can obtain high selectivity of low-carbon olefins in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2006/16C01P2004/03C01P2002/72
Inventor 曾高峰吴平于幸刘国娟刘子玉陈新庆孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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