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Method for synthesizing heteroatom substituted MeAPO-31 molecular sieve by microwave heating

A technology of microwave heating and meapo-31, which is applied in the field of preparation of MeAPO-31 molecular sieve, can solve the problems of long crystallization time, prone to miscellaneous crystals in the product, narrow adjustable range of acidity, and achieve broad application prospects and cost reduction Effect

Inactive Publication Date: 2011-04-06
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the technical problems of long crystallization time in the existing method for preparing MeAPO-31 molecular sieve, miscellaneous crystals are prone to appear in the product, the type and quantity of heteroatoms introduced into the skeleton are limited, and the adjustable range of acid sites produced is narrow, etc. And provide a kind of microwave heating synthetic heteroatom replacement MeAPO-31 (Me refers to heteroatoms such as Mg, Co, Mn, Fe, Cr, Ti, Cu, Zn, V) molecular sieve method

Method used

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  • Method for synthesizing heteroatom substituted MeAPO-31 molecular sieve by microwave heating
  • Method for synthesizing heteroatom substituted MeAPO-31 molecular sieve by microwave heating
  • Method for synthesizing heteroatom substituted MeAPO-31 molecular sieve by microwave heating

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specific Embodiment approach 1

[0008] Specific embodiment one: the method for the synthesis of MeAPO-31 molecular sieve by microwave heating in this embodiment is carried out according to the following steps: one, concentrated phosphoric acid is added in water, stir 5min~10min, continue to stir 10~30min after adding di-n-butylamine, then After adding metal salt and aluminum salt, continue stirring for 1h-8h to obtain a gel, wherein the mass ratio of concentrated phosphoric acid to water is 1:2.5-4, and the mass ratio of concentrated phosphoric acid to di-n-butylamine is 1:0.4-1.2 The mass ratio of concentrated phosphoric acid and metal salt is 1:0.04~1.0, the aluminum salt is aluminum isopropoxide or pseudo-boehmite, the mass ratio of concentrated phosphoric acid and aluminum isopropoxide is 1.2~2, concentrated phosphoric acid and The mass ratio of pseudo-boehmite is 0.2~1.2; 2. The gel obtained in step 1 is placed in a reaction kettle, and microwaves are used as a heating source. The power of the microwaves...

specific Embodiment approach 2

[0011] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the magnesium salt in step one is magnesium acetate or magnesium nitrate, the cobalt salt is cobalt sulfate, cobalt nitrate or cobalt acetate, and the manganese salt is acetic acid Manganese or manganese sulfate, the iron salt is iron nitrate or iron sulfate, the chromium salt is chromium nitrate or chromium acetate, the titanium salt is titanium chloride or n-butyl titanate, and the copper salt is copper nitrate, Copper sulfate or copper chloride, the zinc salt is zinc acetate or zinc sulfate, and the vanadium salt is ammonium vanadate. Other steps and parameters are the same as in the first embodiment.

specific Embodiment approach 3

[0012] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the stirring speed in step 1 is 200 r / min. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention discloses a method for synthesizing a heteroatom substituted MeAPO-31 molecular sieve by microwave heating, relating to a preparation method of a MeAPO-31 molecular sieve. The invention aims to solve the technical problems that the traditional method for preparing the MeAPO-31 molecular sieve has long crystallization time, easy generation of mixed crystals in products, limited type and quantity of the heteroatom introduced into a frameworkd, the narrow adjustable range of the produced acid sites and the like. The method comprises the following steps of: firstly, preparing gel by using phosphoric acid, water, di-n-butylamine, aluminum isopropoxide (or boehmite) and metal salt; heating with microwaves; and crystallizing, then centrifugally filtering, washing, drying and roasting to obtain the MeAPO-31 molecular sieve. Compared with the traditional hydrothermal process, the method disclosed in the invention obviously shortens the crystallization time of the molecular sieve and does not generate mixed crystals. The MeAPO-31 molecular sieve prepared with the method can be used as catalysts in the fields of petrochemical industry, fine chemical industry and the like.

Description

technical field [0001] The invention relates to a preparation method of MeAPO-31 molecular sieve. Background technique [0002] AlPO-31 is composed of AlO 4 with PO 4 Aluminophosphate molecular sieves with an ATO-type topology composed of alternating tetrahedrons have a balanced skeleton charge and no acidic sites. Introduce metal heteroatoms such as Mg, Co, Zn, Ti, Mn, Fe, V into the framework of aluminum phosphate molecular sieve to partially replace Al or P to make heteroatom-substituted MeAPO-31 molecular sieve, which makes the framework of aluminum phosphate molecular sieve exchangeable. The charge can be used as a molecular sieve catalyst with mild acidity. Compared with the silicoaluminophosphate molecular sieve (SAPO-31) with the same topological structure, the MeAPO-31 molecular sieve formed by introducing only a small amount of Mg, Co and other heteroatoms into the AlPO-31 molecular sieve framework can generate abundant active sites, overcoming In the synthesis...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 吴伟杨杰闫鹏飞周亚静
Owner HEILONGJIANG UNIV
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