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A kind of preparation method of mesoporous sapo-34 molecular sieve

A molecular sieve and solution technology, applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of large pore diameter, difficult adjustment of silicon-aluminum ratio, and wide distribution in multi-level porous molecular sieves, to overcome Diffusion bottleneck, low cost of preparation, effect of improving performance

Inactive Publication Date: 2018-04-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, hierarchically porous molecular sieves synthesized using polymers as templates have large mesopore sizes and wide distribution
In addition, Chemical Communication (2009, 3283-3284) also reported the method of using cheap natural layered kaolin to prepare hierarchically porous SAPO-34. The prepared hierarchically porous SAPO-34 is formed by intersecting nanosheets with a thickness of 60nm , where the pores come from the gaps between nanosheets, with a pore size of 30-40nm, but due to the limitation of raw materials, it is difficult to adjust the silicon-aluminum ratio of the product

Method used

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  • A kind of preparation method of mesoporous sapo-34 molecular sieve
  • A kind of preparation method of mesoporous sapo-34 molecular sieve
  • A kind of preparation method of mesoporous sapo-34 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 0.7g of PHAPTMS (density 1.07g / ml), mix it with 3ml of methanol and stir for 5min, slowly add 1ml of deionized water to make a solution; 2 / g gas phase SiO 2 After mixing with 10ml of deionized water and stirring for 5 minutes, it was added to the above solution, heated to 60° C. and stirred for 5 hours at a constant temperature to obtain a silicon source solution.

[0029] Add 20g of TEAOH aqueous solution with a mass concentration of 20% into a beaker, place it in a water bath at 60°C and stir it. After 5ml of water is evaporated, take it out at room temperature, add 2.44g of pseudo-boehmite, stir for 3 hours, and slowly add a mass concentration of 85 %H 3 PO 4 The solution was 2.38ml, stirred for 30 minutes, then added to the silicon source solution and stirred for 2-3 hours to obtain a gel.

[0030] Put the obtained gel into a reaction kettle lined with polytetrafluoroethylene, and conduct a hydrothermal crystallization reaction at 160°C for 10 days. ℃ cal...

Embodiment 2

[0037] Weigh 0.9g of PHAPTMS (density 1.07g / ml), mix it with 3ml of methanol and stir for 5min, slowly add 1ml of deionized water to make a solution; 2 / g gas phase SiO 2 After mixing with 10ml of deionized water and stirring for 5 minutes, it was added to the above solution, heated to 60° C. and stirred for 5 hours at a constant temperature to obtain a silicon source solution.

[0038] Add 23g of TEAOH aqueous solution with a mass concentration of 20% into a beaker, place it in a water bath at 60°C and stir it. After 8ml of water is evaporated, take it out at room temperature, add 2.44g of pseudo-boehmite, stir for 3 hours, and slowly add a mass concentration of 85 %H 3 PO 4 The solution was 2.38ml, stirred for 30 minutes, then added to the silicon source solution and stirred for 2-3 hours to obtain a gel.

[0039] Put the obtained gel into a reaction kettle lined with polytetrafluoroethylene, and conduct a hydrothermal crystallization reaction at 160°C for 10 days. ℃ cal...

Embodiment 3

[0042] Weigh 0.9g of PHAPTMS (density 1.07g / ml), mix it with 3ml of methanol and stir for 5min, slowly add 1ml of deionized water to make a solution; 2 / g gas phase SiO 2 After mixing with 10ml of deionized water and stirring for 5 minutes, it was added to the above solution, heated to 60° C. and stirred for 5 hours at a constant temperature to obtain a silicon source solution.

[0043] Add 20g of TEAOH aqueous solution with a mass concentration of 20% into a beaker, place it in a water bath at 60°C and stir, after evaporating 7ml of water, take it out at room temperature, add 2.44g of pseudo-boehmite, stir for 3 hours, and slowly dropwise add a mass concentration of 85 %H 3 PO 4 The solution was 2.38ml, stirred for 30 minutes, then added to the silicon source solution and stirred for 2-3 hours to obtain a gel.

[0044] Put the obtained gel into a reaction kettle with a polytetrafluoroethylene liner, and conduct a hydrothermal crystallization reaction at 180°C for 6 days. A...

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Abstract

The invention discloses a preparation method of a mesoporous SAPO-34 molecular sieve. The preparation method includes: using PHAPTMS as part of silicon source and a mesoporous hole forming agent for synthesizing the molecular sieve; adding PHAPTMS into raw materials utilizing a microporous template agent TEAOH to synthesize a microporous SAPO-34 molecular sieve; utilizing part of blocking effect, on crystal growing of the molecular sieve, of organic groups in PHAPTMS with coexistence of TEAOH, and directly synthesizing the mesoporous SAPO-34 molecular sieve at one step through hydrothermal crystallization reaction. The mesoporous SAPO-34 molecular sieve prepared by the method is an aggregate uniformly assembled by nanocrystals, and is cuboid-like in appearance, and mesoporous diameter is 2-5 nm.

Description

technical field [0001] The invention relates to a SAPO-34 molecular sieve, in particular to a preparation method of a mesoporous SAPO-34 molecular sieve self-assembled from nanoparticles. Background technique [0002] SAPO-34 molecular sieve is a silicoaluminophosphate crystal material with a chabazite-like structure. Its skeleton structure is composed of double six-membered rings connected by four-membered rings, thus forming an ellipsoidal three-dimensional CHA cage with an eight-membered ring orifice. Pore ​​structure, in which the diameter of the CHA cage is 0.94nm, but the pore size is only 0.38nm. The unique small pore structure of SAPO-34 molecular sieve, as well as its moderate acidity and high thermal / hydrothermal stability, make it suitable for the catalytic reaction of methanol conversion to prepare low-carbon olefins (MTO) and CO 2 / CH 4 and CO 2 / N 2 It shows excellent catalytic performance and separation performance in gas adsorption separation. Especially...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03
Inventor 马静红赵鹏波李瑞丰
Owner TAIYUAN UNIV OF TECH
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