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Preparation method of SAPO-17 molecular sieves

A SAPO-17, molecular sieve technology, applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problem of difficulty in synthesizing SAPO-17 crystals

Inactive Publication Date: 2014-07-16
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the synthesis of SAPO-17 molecular sieve crystals
[0005] So far, it has been reported in the literature that it takes several days to synthesize both AlPO-17 and SAPO-17, and it is difficult to synthesize pure SAPO-17 crystals, and SAPO-35 (LEV) (Zeolites, 1993, Vol13, P549), SAPO-34(CHA) and SAPO-44(CHA) (Crystal Research and Technology, 1994, Vol29, P237) and other impure substances

Method used

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  • Preparation method of SAPO-17 molecular sieves
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  • Preparation method of SAPO-17 molecular sieves

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Embodiment 1

[0030] Embodiment 1: Synthesis of SAPO-17 molecular sieve in situ

[0031] Aluminum isopropoxide was used as the aluminum source, phosphoric acid was used as the phosphorus source, silica sol was used as the silicon source, and cyclohexylamine was used as the template. Aluminum isopropoxide and phosphoric acid were added to ultrapure water and vigorously stirred at room temperature for 2 hours, then cyclohexylamine was added dropwise to the mixed solution, stirred and aged for 2 hours, and then silica sol (30wt% SiO 2 aqueous solution). Al formed 2 o 3 -P 2 o 5 -SiO 2 -CHA-H 2 Each component in the O sol system is according to the molar ratio of oxides:

[0032] P 2 o 5 / Al 2 o 3 = 1,

[0033] CHA / Al 2 o 3 = 1,

[0034] SiO 2 / Al 2 o 3 =0.1,

[0035] h 2 O / Al 2 o 3 =40.

[0036] The aged sol was put into a polytetrafluoroethylene-lined stainless steel reactor and hydrothermally synthesized at 200 °C for 120 h. After the reaction was completed, the reactio...

Embodiment 2

[0038] Embodiment 2: Synthesis of SAPO-17 molecular sieve by seed crystal method (1)

[0039] Aluminum isopropoxide is used as the aluminum source, phosphoric acid is used as the phosphorus source, T-type zeolite is used as the silicon source, and cyclohexylamine is used as the template. Add aluminum isopropoxide and phosphoric acid to ultrapure water and stir vigorously at room temperature for 2 hours, then add 7g of cyclohexylamine dropwise to the mixture and stir for aging for 2 hours, then add spherical T-type zeolite with an average particle size of 100 nanometers to the sol (composed of 6SiO 2 .Al 2 o 3 ). Al formed 2 o 3 -P 2 o 5 -SiO 2 -CHA-H 2 Each component in the O sol system is according to the molar ratio of oxides:

[0040] P 2 o 5 / Al 2 o 3 = 1,

[0041] CHA / Al 2 o 3 = 1,

[0042] SiO 2 / Al 2 o 3 =0.1,

[0043] h 2 O / Al 2 o 3 =40.

[0044] The aged sol was put into a polytetrafluoroethylene-lined stainless steel reactor and hydrothermal...

Embodiment 3

[0046] Embodiment 3: Synthetic SAPO-17 molecular sieve (two) by seed crystal method

[0047] Aluminum isopropoxide is used as the aluminum source, phosphoric acid is used as the phosphorus source, T-type zeolite is used as the silicon source, and cyclohexylamine is used as the template. Add aluminum isopropoxide and phosphoric acid to ultrapure water and stir vigorously at room temperature for 2 hours, then add cyclohexylamine dropwise to the mixed solution and stir for aging for 2 hours, then add spherical T-type zeolite with an average particle size of 100 nm in the sol (composition 6SiO 2 .Al 2 o 3 ). Al formed 2 o 3 -P 2 o 5 -SiO 2 -CHA-H 2 Each component in the O sol system is according to the molar ratio of oxides:

[0048] P 2 o 5 / Al 2 o 3 = 1,

[0049] CHA / Al 2 o 3 = 1,

[0050] SiO 2 / Al 2 o 3 =0.3,

[0051] h 2 O / Al 2 o 3 =40.

[0052] The aged sol was put into a polytetrafluoroethylene-lined stainless steel reactor and hydrothermally synth...

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Abstract

The invention provides a method for synthesizing SAPO-17 molecular sieve crystals. The method is characterized in that high-crystallinity and pure-phase SAPO-17 molecule sieves are quickly synthesized by adopting zeolite molecular sieves (crystalline silicon source) as a silicon source. Compared with a synthesis method adopting amorphous silicon sources such as silica sol and silicon powder, the method is capable of increasing the content of skeleton silicon and greatly increasing the crystallization rate of the molecular sieves; the synthesis time is shortened by 3-10 times. The SAPO-17 molecular sieves synthesized by the method have a weakly acidic activity center and can be used as a catalyst for conversion from methanol into olefins and isomerization of low-carbon hydrocarbon.

Description

technical field [0001] The invention provides a new preparation method of aluminum phosphorus molecular sieve, which belongs to the field of molecular sieve preparation and application. Background technique [0002] AlPOs is a new type of microporous crystal material with an open framework, and it is also the first artificially synthesized molecular sieve that does not contain silicon (patent US4310440). The framework of traditional silicon-alumina molecular sieves is composed of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons, while in most phosphorus-aluminum molecular sieves, aluminum-oxygen tetrahedrons and phosphorus-oxygen tetrahedrons strictly alternate, and the framework is electrically neutral, and there is no exchangeable The cation has no Bronsted acid center on its surface and few Lewis acid sites. However, the skeleton atoms can introduce charges after unequivalent substitution. After introducing heteroatoms Si or metal atoms into the framework of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 陈祥树徐龙女周荣飞张飞桂田胡娜朱美华
Owner JIANGXI NORMAL UNIV
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