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Preparation method for titanium pyrophosphate with flower-like micron/nanometre structure

A nanostructure, titanium pyrophosphate technology, applied in the direction of nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve problems that have not been reported, and achieve the effects of reducing production costs, protecting the environment, and simple processes

Inactive Publication Date: 2013-03-20
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, although there are sporadic reports on the synthesis of nano-titanium pyrophosphate (V.Aravindan, M.V.Reddy, S.Madhavi, S.G.Mhaisalkar, G.V.Subba Rao and B.V.R.Chowdari, J.Power Sources, 2011, 196, 8850-8854.) , but the synthesis of titanium pyrophosphate micro / nanostructures with nano-building blocks has not been reported

Method used

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  • Preparation method for titanium pyrophosphate with flower-like micron/nanometre structure
  • Preparation method for titanium pyrophosphate with flower-like micron/nanometre structure
  • Preparation method for titanium pyrophosphate with flower-like micron/nanometre structure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under the condition of 200r / min stirring, 0.68mmol phytic acid and 2mmol tetrabutyl titanate were added to 80mL absolute ethanol, after stirring evenly, the resulting mixture was transferred to a polytetrafluoro container with a volume of 95mL, and then polytetrafluoroethylene The PTFE container was placed in a stainless steel reaction kettle, and the kettle was sealed; the reaction kettle was kept at 180°C for static heat preservation for 12 hours to obtain a reaction solution. The obtained reaction solution was subjected to solid-liquid separation, and the liquid was recovered for use; the solid was washed with water and alcohol, and dried in an air atmosphere at 60°C for 10 hours to obtain the target product precursor.

[0028] The target product precursor obtained in the above steps was calcined at 680°C for 6 hours to prepare flower-like micro / nanostructured titanium pyrophosphate (sample S-1).

[0029] The XRD result of prepared sample S-1 ( figure 1 , curve (a))...

Embodiment 2

[0032] Under the stirring condition of 400r / min, 2.52mmol of phytic acid and 6mmol of isopropyl titanate were added to 30mL of absolute ethanol. The PTFE container was placed in a stainless steel reaction kettle, and the kettle was sealed; the reaction kettle was kept at 220°C for static heat preservation for 6 hours to obtain a reaction solution. The obtained reaction solution was subjected to solid-liquid separation, and the liquid was recovered for use; the solid was washed with water and alcohol, and dried in an air atmosphere at 120° C. for 6 hours to obtain the target product precursor.

[0033] The target product precursor obtained in the above steps was calcined at 800°C for 1 h to prepare flower-like micro / nanostructured titanium pyrophosphate (sample S-2).

[0034] The XRD result of prepared sample S-2 ( figure 1 , curve (b)) shows that sample S-2 is pure titanium pyrophosphate (JCPDS no.38-1468).

[0035] The scanning electron micrograph of prepared sample S-2 is ...

Embodiment 3

[0037] A preparation method of flower-like micro / nanostructure titanium pyrophosphate, comprising the steps of:

[0038] Under the condition of stirring at 300r / min, 1.4mmol phytic acid and 4mmol titanium tetrachloride were added to 70mL of absolute ethanol, after stirring evenly, the resulting mixture was transferred to a polytetrafluoro container with a volume of 95mL, and then the polytetrafluoroethylene The fluorine container was placed in a stainless steel reaction kettle, and the kettle was sealed; the reaction kettle was kept at 190°C for static heat preservation for 6 hours to obtain a reaction solution. The obtained reaction solution was subjected to solid-liquid separation, and the liquid was recovered for use; the solid was washed with water and alcohol, and dried in an air atmosphere at 70°C for 10 hours to obtain the target product precursor.

[0039]The target product precursor obtained in the above steps was calcined at 750° C. for 2 hours to prepare flower-like...

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Abstract

The invention relates to a preparation method for titanium pyrophosphate with a flower-like micron / nanometre structure, comprising the following steps of: a, adding phytic acid and a titanium source in absolute ethyl alcohol to prepare a mixed solution, and performing heat-insulating reaction on the mixed solution to obtain reaction solution; b, performing solid-liquid separation on the reaction solution, and washing and drying solids to prepare a target product precursor; and c, calcining the target product precursor to prepare the titanium pyrophosphate with the flower-like micron / nanometre structure. Via the preparation method disclosed by the invention, the titanium pyrophosphate with the flower-like micron / nanometre structure is prepared for the first time; and the titanium pyrophosphate with the flower-like micron / nanometre structure has many potential purposes in the fields of bionics, ion exchange, catalysis and lithium battery materials.

Description

technical field [0001] The invention relates to a method for preparing titanium pyrophosphate with a flower-like micro / nano structure, and belongs to the technical field of preparation of titanium pyrophosphate nanomaterials. Background technique [0002] Controlling the size and shape of material particles is a research hotspot and difficulty in the field of material synthesis; because the size and shape of materials, especially nanomaterial particles, have an important impact on their properties (Y.Ma, L.Qi, J . Ma and H. Cheng, Cryst. Growth Des., 2004, 4, 351-354.). Recently, micro / nano materials with secondary structures have attracted great interest of researchers due to their excellent performance in the fields of bionics, gas sensing, catalysis, solar cells and lithium batteries (Y. Zhang, Y. Chen, L. Shi, J. Li and Z. Guo, J. Mater. Chem., 2012, 22, 799-815; H. Jiang, J. Hu, F. Gu, W. Shao and C. Li, Chem .Commun.,2009,3618-3620; Z.Xiong and X.S.Zhao,J.Am.Chem.Soc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/42B82Y40/00
Inventor 盖利刚周艳姜海辉王江彬
Owner QILU UNIV OF TECH
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