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Preparation method for fusiform rod-shaped hexagonal phase BiPO4 powder

A hexagonal phase and rod-shaped technology, which is applied in the field of preparation of spindle-shaped rod-shaped hexagonal phase BiPO4 powder, can solve the problems of no reports, no patents and literature reports, etc., and achieve the effects of environmental friendliness, short reaction time and simple equipment

Active Publication Date: 2015-10-07
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] So far, the preparation of fusiform rod-like hexagonal BiPO 4 The work of powder has not been reported yet, and there are no patents and literature reports on the preparation of fusiform rod-shaped hexagonal BiPO 4 powder

Method used

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  • Preparation method for fusiform rod-shaped hexagonal phase BiPO4 powder
  • Preparation method for fusiform rod-shaped hexagonal phase BiPO4 powder

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Step 1: Bi(NO 3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 O was dissolved in deionized water according to the molar ratio of Bi:P=1:1, and then added (NH 4 ) 2 TiF 6 , prepared as a mixed solution, where (NH 4 ) 2 TiF 6 with Bi(NO 3 ) 3 ·5H 2 The molar ratio of O is 2.0:100,

[0025] Step 2: Add dilute nitric acid with a concentration of 1.2mol / L to adjust the pH value of the mixed solution to be weakly acidic. Stir magnetically at room temperature for 35 minutes until the mixture is evenly mixed to form a precursor solution. The volume ratio of the mixed solution to dilute nitric acid is 46:4 ; Bi(NO 3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 O concentration is 0.07mol / L;

[0026] Step 3: Put the precursor liquid into the microwave hydrothermal reactor lined with polytetrafluoroethylene, and then put the microwave hydrothermal reactor into the microwave hydrothermal reactor MDS-8. The filling ratio of the microwave hydrothermal reactor is 55%, set the microwave power...

Embodiment 2

[0029] Step 1: Bi(NO 3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 O was dissolved in deionized water according to the molar ratio of Bi:P=1:1, and then added (NH 4 ) 2 TiF 6 , prepared as a mixed solution, where (NH 4 ) 2 TiF 6 with Bi(NO 3 ) 3 ·5H 2 The molar ratio of O is 5.0:100,

[0030] Step 2: Add dilute nitric acid with a concentration of 0.5mol / L to adjust the pH value of the mixed solution to be weakly acidic. Stir magnetically at room temperature for 20 minutes until the mixture is evenly mixed to form a precursor solution. The volume ratio of the mixed solution to dilute nitric acid is 45:5 ; Bi(NO3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 The concentration of O is 0.08mol / L;

[0031] Step 3: Put the precursor liquid into the microwave hydrothermal reactor lined with polytetrafluoroethylene, and then put the microwave hydrothermal reactor into the microwave hydrothermal reactor MDS-8. The filling ratio of the microwave hydrothermal reactor is 40%, set the microwave ...

Embodiment 3

[0034] Step 1: Bi(NO 3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 O was dissolved in deionized water according to the molar ratio of Bi:P=1:1, and then added (NH 4 ) 2 TiF 6 , prepared as a mixed solution, where (NH 4 ) 2 TiF 6 with Bi(NO 3 ) 3 ·5H 2 The molar ratio of O is 8.0:100,

[0035] Step 2: Add dilute nitric acid with a concentration of 1.5mol / L to adjust the pH value of the mixed solution to be weakly acidic. Stir magnetically at room temperature for 40 minutes to mix evenly to form a precursor solution. The volume ratio of the mixed solution to dilute nitric acid is 48:2 ; Bi(NO 3 ) 3 ·5H 2 O and Na 3 PO 4 12H 2 O concentration is 0.03mol / L;

[0036] Step 3: Put the precursor liquid into the microwave hydrothermal reactor lined with polytetrafluoroethylene, and then put the microwave hydrothermal reactor into the microwave hydrothermal reactor MDS-8. The filling ratio of the microwave hydrothermal reactor is 60%, set the microwave power of the microwave hy...

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Abstract

The invention provides a preparation method for fusiform rod-shaped hexagonal phase BiPO4 powder. The method comprises the steps that Bi(NO3)3.5H2O, Na3PO4.12H2O and (NH4)2TiF6 serve as raw materials, the raw materials are added into water and stirred evenly, the pH value is regulated to be in faintly acid, and a precursor solution is formed; a microwave hydrothermal method is adopted to enable the precursor solution to be reacted, after the reaction is completed, cooling is performed, sediment in a reaction kettle is taken out, washed and dried, and then the fusiform rod-shaped hexagonal phase BiPO4 powder is obtained. The preparation method for the fusiform rod-shaped hexagonal phase BiPO4 powder has the advantages that devices are simple, and low temperature (about 200 DEG C) and high efficiency (the reaction time is about 60 min) are achieved; the synthesized powder is higher in purity and better in appearance; the preparation method is simple in technology, high in efficiency, low in energy consumption and cost and friendly to environment.

Description

technical field [0001] The invention belongs to the field of functional materials, and relates to a shuttle-shaped rod-shaped hexagonal phase BiPO 4 Powder preparation method. Background technique [0002] As early as the 1980s, a trace amount of colorless bismuth phosphate minerals in microcrystalline, colloidal and earthy aggregates was discovered in the Ximeng tin mining area in Yunnan, my country. Geologists found that the mineral contained 76.34% Bi by analyzing the composition of this mineral. 2 o 3 , 22.92% P 2 o 5 , the crystal chemical formula calculated by P=1 is BiPO 4 . BiPO 4 There are three crystal structure types, monoclinic BiPO 4 , BiPO with monoclinic monazite structure 4 and hexagonal BiPO 4 . BiPO with hexagonal phase structure 4 It can be converted into BiPO with monazite structure above 300°C 4 , can also be transformed into monoclinic BiPO above 600 °C 4 . BiPO with monazite structure 4 It can be transformed into monoclinic BiPO at temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 谈国强折辽娜任慧君夏傲王通
Owner SHAANXI UNIV OF SCI & TECH