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Method of synthesizing super large micropore aluminium phosphate molecular sieve in eutectic mixture

A technology of eutectic mixture and aluminum phosphate molecular sieve, which is applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problem of long crystallization time of molecular sieve, and achieve low synthesis cost, environmental friendliness, low The effect of skeleton density

Inactive Publication Date: 2012-05-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Xu Yunpeng and others disclosed a method for synthesizing aluminum phosphate molecular sieves by microwave heating in Chinese patent CN100410172C. This method adopts the synthesis method of ion heat, and uses microwave radiation as the heating method at the same time, which overcomes the hydrothermal process of conventional aluminum phosphate molecular sieves. Disadvantages such as high pressure process and long crystallization time of molecular sieves

Method used

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  • Method of synthesizing super large micropore aluminium phosphate molecular sieve in eutectic mixture
  • Method of synthesizing super large micropore aluminium phosphate molecular sieve in eutectic mixture
  • Method of synthesizing super large micropore aluminium phosphate molecular sieve in eutectic mixture

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Embodiment 1

[0038] Add 60.0g of tetraethylammonium chloride-pentaerythritol eutectic mixture (TEAC-Pent, TEAC to Pent molar ratio is 0.82:1) into a 100ml beaker, heat up to 100°C, add 6.19g of 85wt% by magnetic stirring Phosphoric acid, 7.6g aluminum isopropoxide, evenly added dropwise 0.96g concentration of 40% hydrofluoric acid, stirred until uniform, then added 1.53g 2-methylimidazole (2-MIm), continued to stir until uniform to obtain the reaction precursor Reactants, where Al 2 o 3 :P 2 o 5 :F - The ratio of :TEAC:2-MIm is 1:1.42:0.53:4.88:0.50 (molar ratio). The above mixture was transferred to a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placed in an oven at 180°C, and kept for 4 hours, then the reaction mixture was cooled to room temperature, 150ml of deionized water was added, stirred, and ultrasonically washed. The reactant was filtered to obtain a white solid powder, which was washed three times repeatedly, and the white powder was washed w...

Embodiment 2

[0042] Add 60.0g of tetraethylammonium chloride-pentaerythritol eutectic mixture (TEAC-Pent, TEAC to Pent molar ratio is 0.41:1) into a 100ml beaker, heat up to 100°C, add 5.23g of 85wt% by magnetic stirring Phosphoric acid, 7.6g aluminum isopropoxide, evenly added dropwise 0.96g concentration of 40% hydrofluoric acid, stirred until uniform, then added 1.53g 2-methylimidazole (2-MIm), continued to stir until uniform to obtain the reaction precursor Reactants, where Al 2 o 3 :P 2 o 5 :F - The ratio of :TEAC:2-MIm is 1:1.20:0.53:2.66:0.50 (molar ratio). The above mixture was transferred to a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placed in an oven at 180°C, and kept for 4 hours, then the reaction mixture was cooled to room temperature, 150ml of deionized water was added, stirred, and ultrasonically washed. The reactant was filtered to obtain a white solid powder, which was washed three times repeatedly, and the white powder was washed w...

Embodiment 3

[0044] 60.0g tetraethylammonium chloride-pentaerythritol eutectic mixture (TEAC-Pent) is added in the 100ml beaker, is warming up to 100 ℃, magnetic stirring adds 7.23g concentration and is the phosphoric acid of 85wt%, 7.6g aluminum isopropoxide, Evenly add 0.96g concentration of 40% hydrofluoric acid, stir until uniform, then add 1.53g 2-methylimidazole (2-MIm), continue stirring until uniform to obtain the reaction precursor reactant, wherein Al 2 o 3 :P 2 o 5 :F - The ratio of :TEAC:2-MIm is 1:1.66:0.53:4.88:0.50 (molar ratio). The above mixture was transferred to a 100ml stainless steel reaction kettle with a polytetrafluoroethylene lining, placed in an oven at 180°C, and kept for 4 hours, then the reaction mixture was cooled to room temperature, 150ml of deionized water was added, stirred, and ultrasonically washed. The reactant was filtered to obtain a white solid powder, which was washed three times repeatedly, and the white powder was washed with 50 ml of acetone....

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Abstract

The invention relates to a method of synthesizing a super large micropore aluminium phosphate molecular sieve in a eutectic mixture. According to the method, the eutectic mixture is used as a medium of a synthesis reaction, and organic amine is added as an auxiliary template, so as to prepare an aluminium phosphate molecular sieve DNL-1 with a CLO structure confirmed by the International Zeolite Association. The preparation method employed by the invention is highly economical, safely and conveniently operated and environment-friendly. The molecular sieve prepared in the invention has good stability, extremely low skeleton density and wide application prospect in catalysis, gas adsorption and separation, etc.

Description

technical field [0001] The invention relates to a synthesis method of ultra-large microporous molecular sieves, in particular to an ion thermal synthesis method of aluminum phosphate molecular sieves with -CLO topological structure. Background technique [0002] Molecular sieves, as the name implies, refer to substances with sieving ability in molecular size. Due to its regular pore structure and unique surface properties, it has been widely used in catalysis, ion exchange, adsorption and separation and other fields. The earliest molecular sieve material recognized by human beings is natural zeolite. In the 1940s, Barrer R M and others realized the artificial synthesis of molecular sieves for the first time. Afterwards, a large number of molecular sieve materials were artificially synthesized one after another. However, with the development of industry, many fields require The performance and structure of molecular sieves put forward higher requirements, so the development ...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 田志坚裴仁彦徐云鹏王磊马怀军王炳春魏莹李科达
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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