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A synthetic method for controllable conversion of indium phosphite into indium phosphate microporous material

A technology of indium phosphate micropores and synthesis methods, which is applied in the field of synthesis of indium phosphite controllable conversion into indium phosphate microporous materials, which can solve the problems of limited application and unsatisfactory performance

Active Publication Date: 2022-08-09
LIAONING TECHNICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In recent years, great progress has been made in the synthesis and performance research of phosphorous acid inorganic microporous materials, and a more abundant and larger pore structure than silicate and phosphate has been obtained. However, due to the thermal stability of phosphorous acid groups, This limits its application in industrial catalysis, gas separation, etc.; phosphoric acid inorganic microporous materials have excellent results in terms of thermal stability, but phosphoric acid groups are inferior to phosphorous acid groups in terms of synthesizing large pore structures. unsatisfactory, therefore, how to achieve both has become a key problem to be solved in this field

Method used

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  • A synthetic method for controllable conversion of indium phosphite into indium phosphate microporous material
  • A synthetic method for controllable conversion of indium phosphite into indium phosphate microporous material
  • A synthetic method for controllable conversion of indium phosphite into indium phosphate microporous material

Examples

Experimental program
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Effect test

example 1

[0031] Mix indium trichloride, deionized water and n-butanol, stir magnetically for 0.5 h, add phosphorous acid to the solution, continue stirring for 1 h, add template 1,2-propanediamine, and finally stir for 2 h to obtain a uniform sol . The molar ratio of the sol is In:P:1,2-Propanediamine:n-Butanol:H 2 O=1.0:10.5:3.5:666.6:44. The obtained sol was allowed to stand for 0.5h, put into a 20ml polytetrafluoroethylene reactor, placed in a 160°C oven for crystallization for 5 days, and the solid product was separated, washed and dried to obtain crystals with a regular dodecahedron shape , does not contain other amorphous substances, such as Figure 4 shown. The obtained crystals were heated to 200 °C in 30 minutes under the protection of industrial nitrogen (oxygen content ≤ 0.5%) atmosphere in a tube furnace, sintered at 200 °C for 2 hours, and then raised to 250 °C for 30 minutes, at 250 °C. ℃ temperature for 2.5 hours, then rise to 300 ℃ through 30 minutes, keep at 300 ℃ ...

example 2

[0033] Mix indium trichloride, deionized water and n-butanol, stir magnetically for 0.5 h, add phosphorous acid to the solution, continue stirring for 1 h, add template 1,2-propanediamine, and finally stir for 2 h to obtain a sol. The molar ratio of the sol is In:P:1,2-Propanediamine:n-Butanol:H 2 O=1.0:10.5:3.5:666.6:44. The obtained sol was allowed to stand for 0.5h, put into a 20ml polytetrafluoroethylene reactor, placed in a 160°C oven for crystallization for 5 days, and the solid product was separated, washed and dried to obtain crystals with a regular dodecahedron shape , does not contain other amorphous substances.

[0034] Under the protection of pure nitrogen (oxygen content ≤ 0.01%) atmosphere in a tube furnace, the obtained crystal was heated to 200 ° C for 30 minutes, sintered at 200 ° C for 2 hours, and then raised to 250 ° C for 30 minutes, at 250 ° C. ℃ temperature for 2.5 hours, then rise to 300 ℃ through 30 minutes, keep at 300 ℃ temperature for 4 hours, and...

example 3

[0036]Mix indium trichloride, deionized water and n-butanol, stir magnetically for 0.5 h, add phosphorous acid to the solution, continue stirring for 1 h, add template 1,2-propanediamine, and finally stir for 2 h to obtain a sol. The molar ratio of the sol is In:P:1,2-Propanediamine:n-Butanol:H 2 O=1.0:10.5:3.5:666.6:44. The obtained sol was allowed to stand for 0.5h, put into a 20ml polytetrafluoroethylene reactor, placed in a 160°C oven for crystallization for 5 days, and the solid product was separated, washed and dried to obtain crystals with a regular dodecahedron shape , does not contain other amorphous substances.

[0037] The obtained crystals were heated to 200 °C in 30 minutes under the protection of industrial nitrogen (oxygen content ≤ 0.5%) atmosphere in a tube furnace, sintered at 200 °C for 2 hours, and then raised to 250 °C for 30 minutes, at 250 °C. Incubate at ℃ for 4h, and then naturally cool, in which the nitrogen gas escape rate is about 90 bubbles per m...

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Abstract

The invention discloses a synthesis method for controllably converting indium phosphite into indium phosphate microporous material. A water / mixed solvothermal method is adopted, phosphorous acid is used as phosphorus source, indium chloride is used as indium source, and 1,2-propanedi Amine is an organic template agent, and n-butanol and deionized water are mixed solvents. According to a certain molar ratio, they are uniformly mixed under magnetic stirring to obtain a sol, which is put into a 20ml polytetrafluoroethylene-lined hydrothermal reactor, and the temperature is 160 ° C. Crystallized under autogenous pressure for 5 days, an indium phosphite microporous compound was obtained; then, the indium phosphite was controllably converted into indium phosphate microporous compounds under the premise of maintaining the pore structure by the method of program-controlled temperature control and atmosphere-controlled heating. Material. The method of the invention provides a new method for synthesizing indium phosphate microporous materials, which can synthesize indium phosphate microporous materials, which are directly sintered and converted into indium phosphite microporous materials and do not contain other impurity phases.

Description

technical field [0001] The invention belongs to the technical field of preparation of phosphate microporous materials, and particularly relates to a synthesis method for controllably converting indium phosphite into indium phosphate microporous materials. Background technique [0002] Phosphate is an important part of inorganic microporous materials. Since the first case of aluminum phosphate reported by U.C.C. Company in 1982, a large number of main group metal phosphate microporous materials have been synthesized. Due to the variability of coordination modes, Its structure ranges from simple zero-dimensional and one-dimensional to complex two-dimensional and three-dimensional. Among the main group phosphate microporous compounds, the indium atom has the largest radius and smaller ionic potential and electronegativity compared with the aluminum and gallium atoms of the same group. The synthesis of indium phosphate microporous materials is relatively difficult, and the resea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/37C01P2004/03C01P2002/72C01P2002/82
Inventor 王学雷吴纯孟超王秋丰洪晓东杨绍斌
Owner LIAONING TECHNICAL UNIVERSITY