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One-step preparation method for hydrogen type multistage pore molecular sieve with SAPO-5 and SAPO-34 symbiosis

A SAPO-34, SAPO-5 technology, applied in the field of inorganic hierarchical porous material preparation, can solve the problems of catalyst deactivation, blocked pores, diffusion, poor mass transfer performance, etc., to reduce costs and reduce steps.

Inactive Publication Date: 2013-04-03
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the MTO (methanol to light olefins) reaction, SAPO-34 is currently the catalyst with the best selectivity for light olefins (ethylene and propylene), but due to its small pores, it leads to poor diffusion and mass transfer performance. Cause rapid carbonization to block the pores and deactivate the catalyst

Method used

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  • One-step preparation method for hydrogen type multistage pore molecular sieve with SAPO-5 and SAPO-34 symbiosis
  • One-step preparation method for hydrogen type multistage pore molecular sieve with SAPO-5 and SAPO-34 symbiosis
  • One-step preparation method for hydrogen type multistage pore molecular sieve with SAPO-5 and SAPO-34 symbiosis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Mix 0.8g of ethyl silicate, 0.1g of STSAC, 20.2g of TEAOH (35% by mass), 8.2g of ground aluminum isopropoxide and 27.0g of deionized water to prepare white slurry liquid A;

[0028] (2) Mix 3.9g of phosphoric acid and 9.0g of deionized water and slowly add dropwise (1mL / min) into liquid A under vigorous stirring (stirring speed is 800r / min);

[0029] (3) Thoroughly stir to obtain uniformly dispersed precursor B, and the molar ratio of the obtained precursor at this time is: 1.0Al 2 o 3 : 1.0P 2 o 5 : 0.19SiO2 2 : 2.4TEAOH : 0.01STSAC : 100H 2 O, then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, and under autogenous pressure, first crystallize at 85°C for 24 hours, and then crystallize at 200°C for 48 hours. After the crystallization is completed, the solid product After suction filtration, washing with deionized water until neutral, and drying in the air at 100°C for 1 day, 2.9 g of the original powder of microporou...

Embodiment 2

[0032] (1) Mix 0.8g of ethyl silicate, 0.1g of STSAC, 20.2g of TEAOH (35% by mass), 8.2g of ground aluminum isopropoxide and 27.0g of deionized water to prepare white slurry liquid A;

[0033] (2) Mix 3.9g of phosphoric acid and 9.0g of deionized water and slowly add dropwise (2mL / min) into liquid A under vigorous stirring (stirring speed is 600r / min);

[0034] (3) Thoroughly stir to obtain uniformly dispersed precursor B, and the molar ratio of the obtained precursor at this time is: 1.0Al 2 o 3 : 1.0P 2 o 5 : 0.19SiO2 2 : 2.4TEAOH : 0.01STSAC : 100H 2 O, then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, and crystallize it at 200°C for 72 hours under autogenous pressure. properties, dried in air at 80°C for 3 days to obtain 3.0 g of hydrogen-form SAPO-5 and SAPO-34 symbiotic microporous-mesoporous composite molecular sieve powder;

[0035](4) The original powder obtained in step (3) was roasted in the air at a heating rate o...

Embodiment 3

[0037] (1) Mix 0.8g of ethyl silicate, 0.1g of STSAC, 8.4g of TEAOH (35% by mass), 8.2g of ground aluminum isopropoxide and 16.8g of deionized water to prepare white slurry liquid A;

[0038] (2) Mix 2.4g of phosphoric acid and 8.4g of deionized water and slowly add dropwise (1mL / min) into liquid A under vigorous stirring (stirring speed is 900r / min);

[0039] (3) Thoroughly stir to obtain uniformly dispersed precursor B, and the molar ratio of the obtained precursor at this time is: 1.0Al 2 o 3 : 0.6P 2 o 5 : 0.19SiO2 2 : 1.0TEAOH: 0.01STSAC: 70H 2 O, then put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, and crystallize it at 180°C for 120 hours under autogenous pressure. properties, dried in air at 100°C for 1 day to obtain 2.1 g of hydrogen-form SAPO-5 and SAPO-34 symbiotic microporous-mesoporous composite molecular sieve powder;

[0040] (4) The original powder obtained in step (3) was roasted in the air at a heating rate of ...

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Abstract

The invention belongs to the technical field of preparation of inorganic multistage pore materials, and relates to a one-step preparation method for a hydrogen type multistage pore molecular sieve with SAPO-5 and SAPO-34 symbiosis. According to the invention, tetraethylammonium hydroxide (TEAOH) is used as atemplate agent, and an organic silicon surface active agent (STSAC) is used at the same time to prepare a hydrogen type micropore-mesopore composite molecular sieve with SAPO-5 and SAPO-34 symbiosis in one step through the hydrothermal method, so that the acid exchange step is avoided, and the cost is reduced. The molecular sieve is used as catalyst for preparing low-carbon olefin with methanol, so that the limitations to aspects of dispersion and mass transfer can be overcome, the caking speed is reduced, the catalysis life is possibly prolonged, and wide application foreground is anticipated in industrial catalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic hierarchical porous materials, and relates to a method for preparing hydrogen-type SAPO-5 and SAPO-34 symbiotic hierarchical porous (micropore-mesoporous composite) molecular sieves in one step. Background technique [0002] Silicoaluminophosphate molecular sieve (SAPO) (US 4440871) is obtained by Si isomorphous substitution of aluminum phosphate series molecular sieve (AIPO), and SAPO-5 and SAPO-34 are its members. SAPO-5 is a silicoaluminophosphate molecular sieve with AEI structure type, which can be used in many fields such as shape-selective catalysis and catalyst carrier. Patent CN 101302015A and patent CN 102372287A both report the preparation method of SAPO-5. SAPO-34 belongs to the crystal structure of chabazite-like (CHA), and the existing preparation methods mainly use organic templates such as tetraethylammonium hydroxide, triethylamine, diethylamine and morpholine to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 王润伟张宗弢蒋尚
Owner JILIN UNIV
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