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Preparation method of mesoporous SAPO-34 molecular sieve

A molecular sieve and solution technology, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of wide distribution, large pore size of multi-stage molecular sieve, difficulty in adjusting the ratio of silicon to aluminum, etc., and achieve improvement performance, overcoming the diffusion bottleneck, and the effect of low preparation cost

Inactive Publication Date: 2016-08-24
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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  • Preparation method of mesoporous SAPO-34 molecular sieve
  • Preparation method of mesoporous SAPO-34 molecular sieve
  • Preparation method of mesoporous SAPO-34 molecular sieve

Examples

Experimental program
Comparison scheme
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 Applications(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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