Synthesis method and application of AEN-structured Si-P-Al molecular sieve

A technology of silicon-phosphorus-aluminum molecular sieve and synthesis method, which is applied in the direction of molecular sieve characteristic silicon-aluminophosphate, molecular sieve and alkali-exchanged phosphate, separation method, etc., can solve the problems such as difficult synthesis of AEN structure silicon-phosphorus-aluminum molecular sieve, and achieve good application prospects , low addition ratio, easy synthesis effect

Active Publication Date: 2018-04-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In summary, the existing technology is easy to synthesize AEN structure aluminum phosphorus molecular sieve, but it is difficult to synthesize AEN structure silicon phosphorus aluminum molecular sieve

Method used

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  • Synthesis method and application of AEN-structured Si-P-Al molecular sieve
  • Synthesis method and application of AEN-structured Si-P-Al molecular sieve
  • Synthesis method and application of AEN-structured Si-P-Al molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] 4.91 g of pseudoboehmite (Al 2 o 3 Massfraction 83%) and 26.58 grams of deionized water are stirred and mixed to evenly, and 9.22 grams of orthophosphoric acid (H 3 PO 4 mass fraction 85%), fully stirred at 60°C, and aged for 18 hours to prepare mixture A. The mixture A was poured into a tray, and dried at 80° C. for 20 hours to obtain a phosphoraluminum xerogel.

[0091] Get 7.59 grams of obtained phosphorus-aluminum dry glue (solid content 80.3%) and add in the polytetrafluoroethylene lining, and add 0.75 grams of silica sol (SiO 2 Mass fraction 30%), 6.86 gram deionized water, 5.77 gram 1-methyl-4-piperidone (C 6 h 11 NO mass fraction 98%), stir evenly, wherein the adding molar ratio of each component is: P 2 o 5 / Al 2 o 3 =1.0, SiO 2 / Al 2 o 3 =0.15, R / Al 2 o 3 =2.0,H 2 O / Al 2 o 3 =20.

[0092] Cover the polytetrafluoroethylene liner with the above reaction mixture, put it into a stainless steel autoclave and seal it, place the autoclave in a rotar...

Embodiment 2

[0095] 4.91 g of pseudoboehmite (Al 2 o 3 Mass fraction 83%) and 34.95 grams of deionized water were stirred and mixed until uniform, and 10.78 grams of ammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 mass fraction 98%), fully stirred at 60°C, and aged for 12 hours to prepare mixture A. The mixture A was poured into a tray, and dried at 80° C. for 24 hours to obtain a phosphoraluminum xerogel.

[0096] Get 7.63 grams of obtained phosphorus-aluminum dry glue (solid content 79.9%) and add in the polytetrafluoroethylene liner, and add 0.48 grams of solid silica gel (SiO 2 Mass fraction 93%), 5.10 gram deionized water, 4.33 gram 1-methyl-4-piperidone (C 6 h 11 NO mass fraction 98%), stir evenly, wherein the adding molar ratio of each component is: P 2 o 5 / Al 2 o 3 =1.0, SiO 2 / Al 2 o 3 =0.3, R / Al 2 o 3 =1.5,H 2 O / Al 2 o 3 =15.

[0097] Cover the polytetrafluoroethylene liner with the above reaction mixture, put it into a stainless steel autoclave and seal it, plac...

Embodiment 3

[0100] 5.44 grams of aluminum hydroxide dry glue (Al 2 o 3 Massfraction 75%) and 29.93 grams of deionized water, stir and mix to uniform, add 7.38 grams of orthophosphoric acid (H 3 PO 4 mass fraction 85%), fully stirred at 70°C, and aged for 12 hours to prepare mixture A. The mixture A was poured into a tray, and dried at 80° C. for 24 hours to obtain a phosphoraluminum xerogel.

[0101] Get 6.51 grams of obtained phosphorus-aluminum dry glue (solid content 82.7%) and add in the polytetrafluoroethylene lining, and add 0.77 grams of white carbon black (SiO 2 Mass fraction 98%), 10.02 gram deionized water, 4.33 gram 1-methyl-4-piperidone (C 6 h 11 NO mass fraction 98%), stir evenly, wherein the adding molar ratio of each component is: P 2 o 5 / Al 2 o 3 =0.8, SiO 2 / Al 2 o 3 =0.5, R / Al 2 o 3 =1.5,H 2 O / Al 2 o 3 =25.

[0102]Cover the polytetrafluoroethylene liner with the above reaction mixture, put it into a stainless steel autoclave and seal it, place the aut...

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Abstract

The invention relates to the field of synthesis of catalytic materials and discloses a synthesis method and an application of an AEN-structured Si-P-Al molecular sieve. The synthesis method comprisesa mode one: a mixed solution containing a P source, an Al source, a Si source, a structure-directing agent and water is subjected to hydrothermal crystallization with a hydrothermal method and then issubjected to solid-liquid separation and dried; a mode two: a mixed solution A containing the P source, the Al source and water is aged and dried with a P-Al dry glue liquid phase conversion method,and dry P-Al glue is prepared; a raw material mixture B containing the dry P-Al glue, the Si source, the structure-directing agent and water is subjected to hydrothermal crystallization, solid-liquidseparation and drying, wherein the structure-directing agent is 1-methyl-4-piperidinone and / or 1,3-dimethyl-4-piperidone. According to the synthesis system, the AEN-structured Si-P-Al molecular sieveis easy to synthesize. The AEN-structured Si-P-Al molecular sieve synthesized with the method can be applied to storage of small molecule gases such as hydrogen, methane and the like, can also be usedfor gas absorption separation and has good application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing the silicon-phosphorus-aluminum molecular sieve with an AEN structure, and also relates to the application of the silicon-phosphorus-aluminum molecular sieve with the AEN structure. Background technique [0002] In 1985, Australian scientist John B. Parise synthesized AlPO-EN3 molecular sieve for the first time. AlPO-EN3 molecular sieves were synthesized under hydrothermal conditions at 200°C using ethylenediamine (EN) as a structure-directing agent. Its chemical formula is Al 6 (PO 4 ) 6 4H 2 O EN, belongs to the orthorhombic crystal system, the space group is P2 1 2 1 2 1 , the unit cell constant is It has a two-dimensional eight-membered ring channel structure, the pore diameter of the eight-membered ring along the [100] direction is 0.43×0.31nm, and the pore diameter of the eight-membered ring along the [010] direction is 0.27×0.50nm, which belongs to small-pore molecular sieves (Studies i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01D53/02
CPCB01D53/02B01D2253/116C01B37/08C01B39/54C01P2002/30C01P2002/72C01P2004/03
Inventor 梁世航张羿王永睿慕旭宏徐广通舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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