Synthesis method of aluminum phosphate molecular sieve with three-dimensional crossed channels

A technology of aluminum phosphate molecular sieve and synthesis method, applied in molecular sieve and alkali exchange phosphate, bulk chemical production and other directions, can solve problems such as a large number of organic acid and alkali waste liquids

Inactive Publication Date: 2011-06-22
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

[0004] This patent overcomes the shortcomings of conventional synthesis of LTA molecular sieves: hydrothermal high-pressure process, a large amount of organic acid-base waste liquid

Method used

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  • Synthesis method of aluminum phosphate molecular sieve with three-dimensional crossed channels
  • Synthesis method of aluminum phosphate molecular sieve with three-dimensional crossed channels

Examples

Experimental program
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Embodiment 1

[0023] Add 30g of 1-butyl-3-methylimidazolium bromide ionic liquid into a 100ml beaker, raise the temperature to 120°C, stir magnetically and add 3.8g of aluminum isopropoxide evenly, drop 0.5g evenly with a mass concentration of 40% hydrofluoric acid, stirred for 2 hours until uniform, dropwise added 2.16g of phosphoric acid with a mass concentration of 85%, then uniformly added 2.1g of di-n-propylamine, continued to stir for 10 minutes, raised the temperature to 160°C, kept stirring for 12 hours, and then The reaction mixture was cooled to room temperature, 50 ml of deionized water was added, stirred, ultrasonically washed, the reactant was filtered to obtain a white solid powder, the washing was repeated three times, and the white was washed with 50 ml of acetone. The final white powder was dried in an oven at 110° C., and tested by XRD, the white powder was AlPO4-42 (LTA structure) molecular sieve, pure phase. The moisture and solvent in the filtrate after washing are evap...

Embodiment 2

[0025] Add 30g of 1-butyl-3-methylimidazolium bromide ionic liquid into a 100ml beaker, raise the temperature to 120°C, stir magnetically and add 3.8g of aluminum isopropoxide evenly, drop 0.5g evenly with a mass concentration of 40% hydrofluoric acid, stirred for 2 hours until uniform, dropwise added 3.34g of phosphoric acid with a mass concentration of 85%, then uniformly added 3.0g of triethylamine, continued to stir for 10 minutes, raised the temperature to 160°C, kept stirring for 24 hours, and then The reaction mixture was cooled to room temperature, 50 ml of deionized water was added, stirred, ultrasonically washed, the reactant was filtered to obtain a white solid powder, the washing was repeated three times, and the white was washed with 50 ml of acetone. The final white powder was dried in an oven at 110° C., and tested by XRD, the white powder was AlPO4-42 (LTA structure) molecular sieve, pure phase. The moisture and solvent in the filtrate after washing are evapora...

Embodiment 3

[0027] Add 25g of 1-butyl-3-methylimidazolium bromide ionic liquid into a 100ml beaker, heat up to 120°C, stir magnetically and add 3.8g of aluminum isopropoxide evenly, drop 0.5g evenly with a mass concentration of 40% hydrofluoric acid, stirred for 2 hours until uniform, dropwise added 2.16g of phosphoric acid with a mass concentration of 85%, then uniformly added 1.8g of n-butylamine, continued to stir for 10 minutes, raised the temperature to 160 ° C, kept stirring for 4 hours, and then The reaction mixture was cooled to room temperature, 50 ml of deionized water was added, stirred, ultrasonically washed, the reactant was filtered to obtain a white solid powder, the washing was repeated three times, and the white was washed with 50 ml of acetone. The final white powder was dried in an oven at 110° C., and tested by XRD, the white powder was AlPO4-42 (LTA structure) molecular sieve, pure phase. The moisture and solvent in the filtrate after washing are evaporated in a rotar...

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Abstract

The invention discloses a synthesis method of an aluminum phosphate molecular sieve with three-dimensional crossed channels, in particular to a solvent thermosynthesis method adopting ionic liquid as a solvent and a template agent. The channel structure of the aluminum phosphate molecular sieve accords with the crystal structure of an LTA (Linde Type A) molecular sieve defined by an IZA (International Zeolite Association); and the aluminum phosphate molecular sieve is provided with the three-dimensional crossed channels and octatomic ring channel windows. The invention overcomes the defects of a hydrothermal high pressure process and a large amount of organic acid-base waste liquor during the conventional synthesis of the LTA molecular sieve; the invention has the synthesis advantages of taking the ionic liquid as the solvent and the template agent and carrying out crystallization reaction under normal pressure; and in addition, the synthesis method provided by the invention is environmental-friendly without discharging acid-base waste liquor in the synthetic process, and the ionic liquid can be repeatedly used.

Description

technical field [0001] The present invention relates to a method for synthesizing a molecular sieve with an LTA structure, more precisely an aluminum phosphate molecular sieve (AlPO4-42) with an LTA structure and a method for synthesizing it in an ionic liquid. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve developed by United Carbide Corporation in the early 1980s after silicon aluminum molecular sieve (USP4310440, the characteristic of this type of molecular sieve is that its skeleton is alternately linked by phosphorus-oxygen tetrahedron and aluminum-oxygen tetrahedron It has a rich skeleton topology and open pore structure, and has a wide range of applications in the fields of gas separation and catalytic reactions. LTA-type aluminum phosphate molecular sieves have three-dimensional intersecting channels, which are formed by SOD cages through double four-membered ring links. The supercage structure of the eight-mem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54
CPCY02P20/54
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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