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Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier

A technology of aluminum phosphate molecular sieve and alumina carrier, which is applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali-exchanged phosphate, phosphorus compound, etc. It can solve the problems of potential safety hazards, heavy and complicated coating process, and environmental pollution, and achieve easy operation , good gas separation and permeability performance, and environmentally friendly effect

Active Publication Date: 2015-04-22
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

The above preparation methods all have certain shortcomings: the in situ synthesis method has relatively strict requirements on the substrate and synthesis conditions; the secondary synthesis method inevitably requires pre-prepared nano-scale molecular sieve crystals as seed crystals, and the coating process is cumbersome and complicated. ; In addition, since these two methods are based on hydrothermal synthesis technology, the self-generated pressure of the system generated during the synthesis process will lead to certain safety hazards; in addition, a large amount of acid-base waste liquid generated during the synthesis process will also cause certain damage to the environment. Pollution

Method used

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  • Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier
  • Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier
  • Preparation of highly oriented AEL aluminophosphate molecular sieve membrane supported by alumina carrier

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Effect test

Embodiment 1

[0030]Add 76.4 grams of 1-ethyl-3-methyl imidazolium bromide ionic liquid into a 100 ml beaker, heat up to 100°C, evenly add 0.5 gram of hydrofluoric acid with a mass concentration of 40%, stir for 2 hours until uniform, and Wherein dropwise adding 2.3 grams of mass concentration is 85% phosphoric acid, P 2 o 5 :F - : The molar ratio of the ionic liquid is 1:1:40, continue to stir for 10 minutes, then pour the reaction solution into the reactor in which the δ-circular sheet-shaped alumina carrier has been placed in advance, and pay attention to the fact that the carrier must be completely immersed in the reaction solution , the dosage ratio of the support body to the precursor reaction solution is 0.5 (cm 2 ·ml -1 surface area of ​​the support), the reactor was heated to 150°C and kept for 12 hours, then the reactor was lowered to room temperature, the support was taken out, ultrasonically washed three times in deionized water, and soaked in acetone for washing. The washed...

Embodiment 2

[0033] Add 76.4 grams of 1-ethyl-3-methylimidazolium bromide ionic liquid into a 100 ml beaker, heat up to 120°C, evenly add 1 gram of hydrofluoric acid with a mass concentration of 40%, stir for 2 hours until uniform, and Wherein dripping 1.15 gram mass concentration is the phosphoric acid of 85%, P 2 o 5 :F - : The molar ratio of the ionic liquid is 1:4:80, continue to stir for 10 minutes, then pour the reaction solution into the reactor in which the δ-circular flake alumina carrier has been placed in advance, and pay attention to the fact that the carrier must be completely immersed in the reaction solution , the dosage ratio of support body to precursor reaction solution is 0.6(cm 2 ·ml -1 surface area of ​​the support), the reactor was heated to 160°C and kept for 24 hours, then the reactor was lowered to room temperature, the support was taken out, ultrasonically washed three times in deionized water, and soaked in acetone for washing. The washed carrier was dried in...

Embodiment 3

[0035] Add 76.4 grams of 1-ethyl-3-methylimidazolium bromide ionic liquid into a 100 ml beaker, heat up to 90°C, evenly add 1 gram of hydrofluoric acid with a mass concentration of 40%, stir for 2 hours until uniform, and Wherein dropping 0.23 gram mass concentration is the phosphoric acid of 85%, P 2 o 5 :F - : The molar ratio of the ionic liquid is 1: 20: 200, continue stirring for 10 minutes, then pour the reaction solution into the reactor in which the θ-square sheet-shaped alumina carrier has been placed in advance, and pay attention that the carrier must be completely immersed in the reaction solution. The dosage ratio of support body and precursor reaction solution is 0.4 (cm 2 ·ml -1 surface area of ​​the support), the reactor was heated to 120°C and kept for 480 hours, then the reactor was lowered to room temperature, the support was taken out, ultrasonically washed three times in deionized water, and soaked in acetone for washing. The washed carrier was dried in ...

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Abstract

The invention specifically relates to a preparation method of a highly C axis oriented AEL structure aluminophosphate molecular sieve membrane supported by a porous alumina carrier. According to the method, an ionic liquid is taken as a reaction medium, and under the auxiliary effect of a mineralizer, the porous alumina carrier reacts with a phosphorus-containing compound, so that the highly C axis oriented AEL structure microporous aluminophosphate molecular sieve membrane can be synthesized on the surface of the alumina carrier. The highly C axis oriented AEL molecular sieve membrane prepared by the method involved in the invention has good gas permeation separation performance. The method provided in the invention is characterized by synthesis of the molecular sieve membrane in the ionic liquid, thus overcoming self-generation of high pressure by the system during conventional hydrothermal synthesis of a molecular sieve membrane. The method involved in the invention has the advantages of environmental-friendliness and simple operation.

Description

technical field [0001] The invention relates to an ionothermal synthesis method of a microporous aluminum phosphate molecular sieve membrane, more precisely relates to an aluminum phosphate molecular sieve membrane with a highly C-axis oriented AEL zeolite structure and a preparation method thereof. Background technique [0002] Molecular sieves are a class of inorganic microporous materials with regular pore structures. For decades, researchers and engineers have been working on the research and synthesis of molecular sieves with different pore characteristics as catalysts for specific chemical reaction processes. With the continuous advancement of science and technology, people gradually realize that if molecular sieves can be prepared into membranes, they can combine the characteristics of molecular sieve materials and film materials to greatly broaden their application fields: using the precise molecular sieving function of molecular sieve micropores At the same time, c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/04
Inventor 田志坚李科达厉晓蕾王磊马怀军徐仁顺王炳春
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI