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Method for preparing zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4

A technology of 3C3N2H4 and C3N2H4, which is applied in the field of preparation of zinc phosphate compounds, can solve the problems of not further exploring the correlation of zinc phosphate compounds and the long time required for synthesis, and achieve uniform morphology, small crystal size and large specific surface area. Effect

Inactive Publication Date: 2015-07-15
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two scientific research teams only reported on the synthesis and structural composition of new zinc phosphate compounds. The synthetic methods used are the traditional hydrothermal method, which takes a long time to synthesize, and did not further explore these two methods. Correlation Between Synthetic Conditions and Structures of Zinc Phosphate Compounds

Method used

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  • Method for preparing zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4
  • Method for preparing zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4
  • Method for preparing zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4

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Effect test

Embodiment 1

[0046] Preparation of zinc phosphate compound Zn(C 3 N 2 h 4 )HPO 4 The method includes the following steps:

[0047] (1) Add zinc acetate with a mass fraction of 99%, imidazole with a mass fraction of 99%, and phosphoric acid with a mass fraction of 85% into deionized water in sequence, and magnetically stir for 2 hours at a speed of 300r / min to obtain the initial mixing solution;

[0048] The mol ratio that the zinc acetate of 99% and the phosphoric acid of 85% is that the massfraction is 1:1.0; The mol ratio that the zinc acetate of 99% and the imidazole that massfraction is 99% is 1: 3.0; the mass fraction is 99% zinc acetate and the molar ratio of deionized water is 1:70;

[0049](2) Place the initial mixed solution obtained in step (1) in a special microwave reactor made of polytetrafluoroethylene, with a heating power of 400W, crystallize at 140°C for 90min, and cool naturally to room temperature to obtain Crystallize the product, then wash the crystallized produc...

Embodiment 2

[0052] Preparation of zinc phosphate compound Zn(C 3 N 2 h 4 )HPO 4 The method includes the following steps:

[0053] (1) Add zinc acetate with a mass fraction of 99%, imidazole with a mass fraction of 99%, and phosphoric acid with a mass fraction of 85% into deionized water in sequence, and magnetically stir for 2 hours at a speed of 300r / min to obtain the initial mixing solution;

[0054] The mol ratio that the zinc acetate of 99% and the phosphoric acid of 85% is that the massfraction is 1:1.0; The mol ratio that the zinc acetate of 99% and the imidazole that massfraction is 99% is 1: 3.0; the mass fraction is 99% zinc acetate and the molar ratio of deionized water is 1:70;

[0055] (2) Place the initial mixed solution obtained in step (1) in a special microwave reactor made of polytetrafluoroethylene, with a heating power of 600W, crystallize at 160°C for 30min, and cool naturally to room temperature to obtain Crystallize the product, then wash the crystallized produ...

Embodiment 3

[0058] Preparation of zinc phosphate compound Zn 4 P 3 o 11 (OH)·3C 3 N 2 h 4 The method includes the following steps:

[0059] (1) Add zinc acetate with a mass fraction of 99%, imidazole with a mass fraction of 99%, and phosphoric acid with a mass fraction of 85% into deionized water in sequence, and magnetically stir for 2 hours at a speed of 300r / min to obtain the initial mixing solution;

[0060] The mol ratio that the zinc acetate of 99% and the phosphoric acid of 85% is that the massfraction is 1:1.0; The mol ratio that the zinc acetate of 99% and the imidazole that massfraction is 99% is 1: 3.0; the mass fraction is 99% zinc acetate and the molar ratio of deionized water is 1:70;

[0061] (2) Place the initial mixed solution obtained in step (1) in a special microwave reactor made of polytetrafluoroethylene, with a heating power of 400W, crystallize at 180°C for 180min, and cool naturally to room temperature to obtain Crystallize the product, then wash the cryst...

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Abstract

The invention discloses a method for preparing zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4, which comprises the following steps: (1) sequentially adding zinc acetate, iminazole and phosphoric acid into deionized water, and magnetically stirring to obtain an initial mixed solution; and (2) putting the initial mixed solution obtained in the step (1) into a special microwave reaction kettle prepared from polytetrafluoroethylene, crystallizing, naturally cooling to room temperature to obtain a crystallization product, washing the crystallization product with deionized water, and drying to obtain the zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4. A microwave heating process is utilized to respectively prepare the zinc phosphate compounds Zn(C3N2H4)HPO4 and Zn4P3O11(OH).3C3N2H4 in one reaction system by changing the reaction conditions.

Description

technical field [0001] The present invention relates to the preparation method of zinc phosphate compound, particularly zinc phosphate compound Zn(C 3 N 2 h 4 )HPO 4 and Zn 4 P 3 o 11 (OH)·3C 3 N 2 h 4 method of preparation. Background technique [0002] Since transition elements successfully entered the framework of molecular sieves such as aluminum phosphate as heteroatoms, the synthesis of transition metal phosphate microporous compounds has attracted more and more people's interest. Since the chemistry of transition metal elements involves redox reactions, photochemical reactions, free radical chemistry and other fields, it is of great significance to synthesize inorganic solid materials with transition metal elements as the skeleton. Among transition metal phosphate microporous compounds, zinc phosphate exhibits rich structural and compositional chemistry. A series of zinc phosphates containing 16-membered rings, 20-membered rings, and 24-membered rings with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C01B25/37C01B25/40
Inventor 宋宇董卉
Owner DALIAN POLYTECHNIC UNIVERSITY
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