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Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve

An aluminum phosphate molecular sieve and multi-stage pore technology, which is applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, can solve the problems of imperfect preparation methods of multi-stage pore molecular sieves, long crystallization time of molecular sieves, etc., and achieve The effect of low synthesis cost, environmental friendliness, safe and convenient operation

Inactive Publication Date: 2016-07-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Disclosed in CN100410172C is the method for synthesizing aluminum phosphate molecular sieve by microwave heating, this method adopts the synthesis method of ionic heat, simultaneously uses microwave radiation as heating mode, has overcome the hydrothermal high-pressure process in conventional aluminum phosphate molecular sieve hydrothermal synthesis process, molecular sieve crystallization Disadvantages such as long time
However, so far, the preparation method of hierarchical porous molecular sieves is not perfect, and there is no report of ionothermal synthesis of hierarchical porous AFI structure aluminum phosphorus molecular sieves.

Method used

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  • Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve
  • Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve
  • Preparation method of hierarchical pore AFI structured aluminum phosphate molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0034]At 90°C, 16.5g of 1-butyl-3-methylimidazolium bromide ionic liquid, 0.44g of aluminum isopropoxide, 0.05g of hydrofluoric acid with a concentration of 40wt%, and 0.75g of phosphoric acid with a concentration of 85wt% were mixed, 0.5 g of n-propylamine was stirred until uniform to obtain a pre-reaction mixture. The reaction mixture was transferred to a stainless steel reaction kettle with a polytetrafluoroethylene liner, and then placed in a 150°C oven for crystallization. After 10 hours of crystallization, the reaction kettle was cooled, and then 150ml of deionized water was added to the reaction mixture. Stir, ultrasonically wash, filter the reactant to obtain a white solid powder, repeat the washing three times, and wash the white powder with 50ml of ethanol. The final white powder was dried in an oven at 110°C, and it was confirmed by XRD test that the white powder was the original powder of aluminum phosphate molecular sieve with AFI structure. The moisture and solv...

Embodiment 2

[0036] At 80°C, 33g of 1-butyl-3-methylimidazolium bromide ionic liquid, 0.88g of aluminum isopropoxide, 1.5g of phosphoric acid with a concentration of 85wt%, 0.05g of hydrofluoric acid with a concentration of 40wt%, and 0.4g Ethanolamine was mixed and stirred until uniform to obtain a pre-reaction mixture. The reaction mixture was transferred to a stainless steel reaction kettle with a polytetrafluoroethylene lining, and then placed in a 150°C oven for crystallization. After crystallization for 6 hours, it was taken out, the reaction kettle was cooled, and then 200ml of deionized water was added to the reaction mixture. Ultrasonic washing was performed, and the reactant was filtered to obtain a white solid powder. The washing was repeated three times, and the white powder was washed with 50 ml of ethanol. The final white powder was dried in an oven at 110°C. It was determined by XRD that the white powder was the original powder of aluminum phosphate molecular sieve with AFI ...

Embodiment 3

[0038] At 80°C, 20g of 1-butyl-3-methylimidazolium bromide ionic liquid, 1.0g of aluminum isopropoxide, 1.8g of phosphoric acid with a concentration of 85wt%, 0.05g of hydrofluoric acid with a concentration of 40wt%, and 0.5g Ethanolamine was mixed and stirred until uniform to obtain a pre-reaction mixture. The reaction mixture was transferred to a stainless steel reaction kettle with a polytetrafluoroethylene liner, and then placed in a 160°C oven for crystallization. After crystallization for 4 hours, the reaction kettle was cooled, and then 300ml of deionized water was added to the reaction mixture. Ultrasonic washing was performed, and the reactant was filtered to obtain a white solid powder. The washing was repeated three times, and the white powder was washed with 50 ml of ethanol. The final white powder was dried in an oven at 110°C. It was confirmed by XRD test that the white powder was the original powder of magnesium aluminum phosphate molecular sieve with AFI struct...

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Abstract

The invention relates to a preparation method of a hierarchical pore AFI structured aluminum phosphate molecular sieve. A macropore-mesopore-micropore composite hierarchical pore aluminum phosphate AFI molecular sieve carrier is prepared through adopting an ionothermal synthesis technology. The molecular sieve synthesis process is carried out under normal pressure or a low self-generated pressure, crystallization conditions are mild, and an ionic liquid can be recovered and repeatedly used, so the method has the advantages of low synthesis cost, no discharge of acids, alkalis or waste liquids in the synthesis process, and environmental protection. The hierarchical pore AFI structured aluminum phosphate molecular sieve prepared in the invention, including macropores, mesopores and micropores, has potential application values in the fields of catalysis, adsorption and separation.

Description

technical field [0001] The invention relates to a preparation method of a multi-level porous AFI structure aluminum phosphate molecular sieve, in particular to a method for synthesizing a multi-level hole AFI structure aluminum phosphate molecular sieve compounded with macropores, mesopores and micropores. Background technique [0002] AFI Structure Aluminum Phosphate Molecular Sieve ( http: / / www.iza-structure.org / databases / ) has a one-dimensional elliptical twelve-membered ring straight channel with a pore size of 0.73nm×0.73nm, and the molecular sieve has good catalytic and separation properties. [0003] Patent CN1388062A discloses a method for synthesizing chromium-phosphorus-aluminum molecular sieve with AFI structure. This method mainly introduces chromium atoms into the framework of molecular sieve with AFI structure. The molecular sieve can be used in the decomposition of cycloalkyl or cycloalkenyl peroxides . LiBaojun (NewJ.Chem., 2014, 38, 3078—3083) reported a ...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 徐仁顺田志坚马怀军王炳春曲炜李鹏潘振栋王从新
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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