SAPO-34 (Silicoaluminophosphate-34) molecular sieve catalyst and application thereof to preparation of low-carbon olefin from methanol

A SAPO-34 and molecular sieve technology, applied in the field of molecular sieves, can solve the problems of molecular sieve crystal size and morphology not uniform, long processing and synthesis time, expensive gel raw materials, etc., to achieve economical solvent consumption, clear morphology and high yield high effect

Inactive Publication Date: 2012-12-26
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2010, Hirota et al. (Mater.Chem.Phys.123(2010)507) synthesized SAPO-34 molecular sieves with an average crystal size of 75 nm by using TEAOH as a template by dry gel conversion method, but this method obtained molecular sieve crystal size and The shape is not uniform
It should be noted that although Top.Catal.19 (2010) 1304 mentions the preparation of nano-sized SAPO-34 molecular sieves and corresponding morphology SAPO-34 molecular sieves, the gel raw materials used in the production method provided are more expensive and the synthesis time is longer And molecular sieve yield is low

Method used

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  • SAPO-34 (Silicoaluminophosphate-34) molecular sieve catalyst and application thereof to preparation of low-carbon olefin from methanol
  • SAPO-34 (Silicoaluminophosphate-34) molecular sieve catalyst and application thereof to preparation of low-carbon olefin from methanol
  • SAPO-34 (Silicoaluminophosphate-34) molecular sieve catalyst and application thereof to preparation of low-carbon olefin from methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Mix and stir tetraethyl orthosilicate, aluminum isopropoxide, water, and tetraethylammonium hydroxide and treat at 20°C for 36 hours under autogenous pressure (closed container) to obtain a mixture; add phosphoric acid to the above mixture, Stirring treatment under autogenous pressure for 12 hours to obtain the initial gel mixture of SAPO-34 molecular sieve; the molar ratio of each component oxide, tetraethylammonium hydroxide and solvent in the initial gel mixture in the reaction system is 3.5TEAOH:0.5 SiO 2 : 1.8P 2 o 5 :Al 2 o 3 : 150H 2O: Put the initial gel mixture into a microwave reactor, heat it up to 160°C under a power of 1000 watts, and carry out constant temperature crystallization under autogenous pressure for 0.5 hours. Then, the solid product was separated by standing, washed with deionized water until neutral, and dried in the air at room temperature to obtain the original powder of SAPO-34 molecular sieve, which was roasted at 550°C for 6 hours to ...

Embodiment 2

[0040] Mix and stir tetraethyl orthosilicate, alumina, water, and tetraethylammonium hydroxide, and then treat it at 20°C under autogenous pressure for 36 hours to obtain a mixture; add phosphoric acid to the above mixture, and stir under autogenous pressure After 12 hours, the initial gel mixture of SAPO-34 molecular sieve was obtained; the molar ratio of each component oxide, tetraethylammonium hydroxide and solvent in the initial gel mixture in the reaction system was 3.5TEAOH:0.5SiO 2 : 1.8P 2 o 5 :Al 2 o 3 : 150H 2 O: Put the obtained initial gel mixture into a polytetrafluoroethylene-lined stainless steel autoclave, statically place it in a 160°C oven (hydrothermal heating), and carry out constant temperature crystallization under autogenous pressure for 120 hours. Then, the solid product was separated by standing, washed neutral with deionized water, and dried in the air to obtain the original powder of SAPO-34 molecular sieve. The original powder was roasted at 550...

Embodiment 3

[0042] Mix and stir tetraethyl orthosilicate, aluminum isopropoxide, water, tetraethylammonium hydroxide and treat at 20°C for 36 hours under autogenous pressure to obtain a mixture; add phosphoric acid to the above mixture, under autogenous pressure Stir for 12 hours to obtain the initial gel mixture of SAPO-34 molecular sieve; the molar ratio of each component oxide, tetraethylammonium hydroxide and solvent in the initial gel mixture in the reaction system is 3.5TEAOH:0.5SiO 2 : 1.8P 2 o 5 :Al 2 o 3 : 60H 2 O: Put the initial gel mixture into a microwave reactor, heat it to 180° C. under a power of 200 watts, and carry out constant temperature crystallization for 1 hour under autogenous pressure. Then, the solid product is centrifuged, washed with deionized water, and dried in the air at room temperature to obtain the original powder of SAPO-34 molecular sieve. The original powder is roasted at 550 ° C for 6 hours to remove the organic ammonium template to obtain SAPO -...

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Abstract

The invention belongs to the technical field of molecular sieve, and particularly relates to an SAPO-34 (Silicoaluminophosphate-34) molecular sieve catalyst and application thereof to preparation of low-carbon olefin from methanol. The spherical SAPO-34 molecular sieve agglomerated by nanoparticles is synthesized by modulating reaction initial gel concentration, and the size range is within a range of 0.5 micron to 10 microns. Tetraethylammonium hydroxide is used as a template and is mixed with an aluminum source, a silicon source and a phosphorus source; the gel concentration is controlled by adding a specific amount of solvent; and the catalyst is quickly prepared by the conventional hydrothermal or microwave heating mode. The spherical SAPO-34 molecular sieve provided by the invention has the characteristics of quickness in production, low cost in gel synthesis raw materials, low reaction energy consumption, high molecular sieve yield and the like. The characteristic of microspheres agglomerated by the nanoparticles enables long life of catalytic application of the nanoparticles, the characteristic of a catalytic effect of the molecular sieve in catalytic reaction can be obviously improved, and meanwhile, the molecular sieve catalyst also has the advantage of easiness in separation and extraction after synthesis of a micron scale catalyst.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to a SAPO-34 molecular sieve catalyst and its application in the production of light olefins from methanol. Background technique [0002] In 1984, United Carbide Corporation (UCC) developed a silicon-substituted aluminum phosphate series S-APO molecular sieve (USP4440871). This type of molecular sieve is a crystalline silicoaluminophosphate, and its three-dimensional skeleton structure is composed of PO 2 + , AlO 2 - and SiO 2 tetrahedron composition. Among them, SAPO-34 is a chabazite-like structure with an ellipsoidal cage composed of an oxygen eight-membered ring and a three-dimensional channel structure, and the orifice is 0.38nm×0.38nm. The suitable pore structure and acidity of SAPO-34 molecular sieve, large specific surface area, good adsorption performance, thermal stability and hydrothermal stability make it show excellent catalytic performance in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/85C07C1/20C07C11/02C07C11/04C07C11/06
CPCY02P20/52Y02P30/20Y02P30/40
Inventor 于吉红杨国炬徐如人
Owner JILIN UNIV
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