Phosphorous acid titanium with three-dimensional open-framework structure and preparation method thereof

A technology of skeleton structure and phosphorous acid, which is applied in phosphorous acid, phosphorus oxyacids, chemical instruments and methods, etc., can solve the problems that artificially synthesized titanium phosphite open skeleton materials have not been reported, and achieve the effect of good thermal stability

Inactive Publication Date: 2014-12-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, to the best of our knowledge, the artificial synthesis of titanium phosphite open-framework materials has not been reported so far.

Method used

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  • Phosphorous acid titanium with three-dimensional open-framework structure and preparation method thereof
  • Phosphorous acid titanium with three-dimensional open-framework structure and preparation method thereof
  • Phosphorous acid titanium with three-dimensional open-framework structure and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A new three-dimensional open framework titanium phosphite structure was synthesized using titanium powder, phosphorous acid, and water as solvents.

[0032] Add 0.24g of titanium powder to a 25mL beaker, continue to add 7mL of water to the beaker and stir for 10 minutes to make it evenly mixed; then add 3.69g of phosphorous acid, continue to stir for 30 minutes to completely dissolve, then transfer the reaction solution to a 15mL poly In a stainless steel kettle lined with tetrafluoroethylene, finally seal the reaction kettle and put it into a 170°C oven for heating for 7 days;

[0033] After the reaction is completed, take out the reaction kettle and let it cool naturally at room temperature; remove the product, wash it repeatedly with deionized water for 6 times, and dry it at 80°C to obtain a new type of three-dimensional open framework titanium phosphate crystal, which is a cuboid Shape, mass about 0.65g.

Embodiment 2

[0035] A new three-dimensional open framework titanium phosphite structure was synthesized with titanium powder, phosphorous acid, hydrofluoric acid, and water as solvents.

[0036] Add 0.24g of titanium powder to a 25mL beaker, continue to add 7mL of water to the beaker and stir for 10 minutes to mix evenly; then add 3.69g of phosphorous acid; continue to stir for 30 minutes to completely dissolve, then add 0.2mL of mass to the beaker The hydrofluoric acid solution with a fraction of 40% was stirred for 30 minutes, then the reaction solution was transferred to a stainless steel kettle lined with 15mL polytetrafluoroethylene, and finally the reaction kettle was sealed and placed in an oven at 170°C for 7 days;

[0037] After the reaction was completed, the reactor was taken out and allowed to cool naturally at room temperature; the product was removed, ultrasonically washed six times with deionized water, and dried at 80°C to obtain a new type of three-dimensional open framewor...

Embodiment 3

[0039] Titanium powder, aqueous solution of phosphorous acid with a mass fraction of 30%, anhydrous piperazine, and water were used as solvents to synthesize a new three-dimensional open framework titanium phosphite structure.

[0040] Add 0.24g of titanium powder into a 25mL beaker, continue to add 7mL of water to the beaker and stir for 10 minutes to make it evenly mixed; then add 6.25mL of an aqueous solution of phosphorous acid with a mass fraction of 30%; continue to stir for 30 minutes, then Add 0.43g of anhydrous piperazine, continue to stir for 30 minutes, then transfer the reaction solution to a stainless steel kettle lined with 15mL polytetrafluoroethylene, and finally seal the reaction kettle and heat it in an oven at 170°C for 7 days;

[0041] After the reaction is completed, take out the reaction kettle and let it cool naturally at room temperature; remove the product, wash it repeatedly with deionized water for 6 times, and dry it at 80°C to obtain a new type of t...

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Abstract

The invention provides phosphorous acid titanium with a three-dimensional open-framework structure and a preparation method thereof and belongs to the technical field of phosphorous acid titanium with a three-dimensional open-framework structure. The preparation method is characterized in that an open-framework crystal compound of the phosphorous acid titanium without an organic template is synthesized by adopting a strong acid method in a hydrothermal system, the morphology of a product is regulated and controlled by adjusting the quantities of phosphorous acid and hydrofluoric acid in reaction gel, and the phosphorous acid titanium compounds with the three-dimensional open-framework structure, which have the identical structure and are different in morphologies, are synthesized. The phosphorous acid titanium compound does not contain an organic template agent. Compared with other metal phosphorous acid salts, the phosphorous acid titanium compound has relatively good heat stability, thus favorable conditions are provided for the research of the property of the phosphorous acid titanium compound. The photovoltage research shows that the compound has the property of a p-type conductor. The invention has the beneficial effects of providing a simple, convenient and effective method for preparing the phosphorous acid titanium crystal material with the open-framework structure.

Description

technical field [0001] The invention belongs to the technical field of titanium phosphite with a three-dimensional open skeleton structure, and in particular relates to a titanium phosphite with an open skeleton structure prepared by a strong acid method and a preparation method thereof. Background technique [0002] Inorganic microporous materials represented by molecular sieves are not only widely used in the fields of catalysis, adsorption, and separation, but also in functional material assembly and drug embedding due to their wide range of internal pore size distribution and rich and diverse topological structures. Show broad application prospects. In recent years, with the development of science and technology, the application of molecular sieves in some emerging fields such as host-guest chemistry, microelectronic devices, optics, and medicine has been gradually developed. Therefore, the preparation of inorganic microporous materials has become one of the research ho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/00C01B25/163
Inventor 李激扬吴俊标刘航
Owner JILIN UNIV
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