Method for preparing AlPO4 or SAPO molecular sieve

A technology of molecular sieve and methyl imidazolium ion, applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve characteristic silicoaluminophosphate, phosphorus compound, etc., can solve the problem of difficult to obtain pure-phase products, and achieve the effect of improving selectivity

Inactive Publication Date: 2006-10-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the synthesis process, a mixture of molecular sieves with different structures is often obtained, and sometimes it is difficult to improve the selectivity of a certain product by adjusting the reaction conditions, so that it is difficult to obtain a pure phase product

Method used

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  • Method for preparing AlPO4 or SAPO molecular sieve
  • Method for preparing AlPO4 or SAPO molecular sieve
  • Method for preparing AlPO4 or SAPO molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 0.5g of n-dipropylamine was added to a round bottom flask containing 40g of 1-butyl-3-methylimidazolium bromide ionic liquid, and 1.0g of 85% H was added at 60°C with stirring 3 PO 4 After stirring for 30 minutes, 1.0 g of aluminum isopropoxide was added, and after stirring for 30 minutes, 0.5 g of 15% HF was added.

[0029] Transfer the round-bottomed flask containing the reaction mixture to an oil bath and heat up to 200° C., continue to stir and react for 1 hour, take out the reactor and cool to room temperature, and filter out the solid sample. The solid sample was washed repeatedly with acetone and water and dried at 100°C. Then the molecular sieve powder was calcined at 550°C in an air atmosphere for 8 hours to obtain AlPO 4 Molecular sieve. After the filtrate was rotary evaporated, it was recrystallized with dichloromethane for the next use.

[0030] The XRD spectrum of the obtained sample is as figure 1 As shown, its crystal phase is the same as AlPO obtain...

Embodiment 2

[0032] 0.4g of triethylamine was added to a round bottom flask containing 30g of 1-hexyl-3-methylimidazolium bromide ionic liquid, and 1.0g of 85% H was added at 70°C with stirring 3 PO 4 After stirring for 30 minutes, 1.0 g of aluminum isopropoxide was added, and after stirring for 30 minutes, 0.5 g of 15% HF was added.

[0033] The round-bottomed flask containing the reaction mixture was transferred to an oil bath and heated to 150° C., and the reaction was continued to stir for 2 hours. The reactor was taken out and cooled to room temperature, and the solid sample was filtered out. The solid sample was washed repeatedly with acetone and water and dried at 100°C. Then the molecular sieve powder was calcined at 550°C in an air atmosphere for 8 hours to obtain AlPO 4 Molecular sieve. After the filtrate was rotary evaporated, it was recrystallized with dichloromethane for the next use.

[0034] The XRD spectrum of the obtained sample is similar to the XRD spectrum of the sa...

Embodiment 3

[0036] 0.4g of triethylamine was added to a round bottom flask containing 30g of 1-butyl-3-methylimidazolium bromide ionic liquid, and 1.0g of 85% H was added at 70°C with stirring 3 PO 4 After stirring for 30 minutes, 1.5 g of aluminum isopropoxide was added, and after stirring for 20 minutes, 0.5 g of 15% HF was added.

[0037] The round bottom flask containing the reaction mixture was transferred to an oil bath and the temperature was raised to 220° C., and the reaction was continued to stir for 3 hours. The reactor was taken out and cooled to room temperature, and the solid sample was filtered out. The solid sample was washed repeatedly with acetone and water and dried at 100°C. Then the molecular sieve powder was calcined at 550°C in an air atmosphere for 8 hours to obtain AlPO 4 Molecular sieve. After the filtrate was rotary evaporated, it was recrystallized with dichloromethane for the next use.

[0038] The XRD spectrum of the obtained sample is as figure 2 As sh...

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Abstract

The invention is a method for preparing AlPO4 or SAPO molecular sieve, using ionic liquid as reaction medium, adding in amine as auxiliary template. And it can be used to synthesize molecular sieves of various structures, comprising the steps of: A) using halogen 1-alkyl-3- methylimidazole ionic liquid as reaction medium and amine as auxiliary template, blending at 70-100 deg.C for 1-30 min; B) adding in precursor compounds of P, Al and Si and hydrofluoric acid to prepare precursor mixture of molecular sieve, crystallizing at 150-300 deg.C for 0.5-3 h, where the molar ratio of Al2O3 to P2O5 to SiO2 to HF to amine to halogen 1-alkyl -3-methylimidazole ionic liquid = 1:(1.7-3.8):(0-1):(0.05-0.2):(0.5-3):(10-40); and C) cooling to room temperature, filtering, washing and drying, so as to obtain a solid-AlPO4 or SAPO molecular sieve.

Description

technical field [0001] The invention discloses a preparation method of a molecular sieve, specifically, using an ionic liquid as a reaction medium and adding an amine as an auxiliary template to prepare AlPO 4 Or the method of SAPO molecular sieve. Background technique [0002] Molecular sieves have been widely studied and applied in many fields for a long time because of their special properties, such as ion exchange, diffusion and adsorption, shape selectivity and catalytic activity. For example, in today's industrial catalysts, molecular sieves are the most widely used type of catalysts. This is mainly due to their unique pore structure, acidity and adsorption properties. The synthesis of molecular sieves with new structures and the development of new molecular sieve synthesis methods have always been the focus of researchers' work. [0003] The traditional synthesis methods of molecular sieves mainly include hydrothermal synthesis and solvothermal synthesis. Syntheti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/04C01B37/08
Inventor 田志坚王磊徐竹生徐云鹏魏莹王炳春林励吾
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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