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Preparation technology of hafnium tetrafluoride

The technology of hafnium tetrafluoride and preparation process is applied in the preparation field of hafnium tetrafluoride, and can solve the problems of high reaction temperature, large difference in oxygen content of products, complicated device, etc., and achieves simple operation process and simple fluorination device. , the effect of low oxygen content

Inactive Publication Date: 2012-11-14
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the dry fluorination method includes hydrogen fluoride (HF) gas fluorination method and ammonium bifluoride (NH 4 HF 2 ) fluorination method, the reaction temperature of hydrogen fluoride gas fluorination method is high, the operation risk is high, and tail gas recovery is difficult; NH 4 HF 2 The method is relatively safe to operate, and the specific method is to use HfO 2 React with ammonium bifluoride under heating conditions to obtain HfF 4 , but the fluorination reaction device is relatively complicated, and requires a high-temperature deamination step, and the oxygen content of the product varies greatly with the process conditions; the wet fluorination method mainly uses hydrofluoric acid precipitation to obtain HfF 4 , the operation is simple and safe, but there is no wet preparation of HfF in the open literature 4 detailed report of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation process of hafnium tetrafluoride, the process includes the following steps:

[0019] (1) Place metal hafnium in hydrofluoric acid to obtain a hafnium tetrafluoride solution;

[0020] (2) Evaporate the hafnium tetrafluoride solution to dryness;

[0021] (3) The hafnium tetrafluoride obtained in step (2) is placed in a quartz tube and dehydrated under vacuum and high temperature conditions to obtain solid hafnium tetrafluoride.

[0022] Using this method, HfF with high purity and low oxygen content was obtained 4 .

Embodiment 2

[0024] Prepare HfF 4 The method includes:

[0025] (1) Put metal hafnium in a polytetrafluoroethylene beaker and add 1% excess hydrofluoric acid, then cover the beaker with filter paper, the metal hafnium and hydrofluoric acid react to obtain a hafnium tetrafluoride solution, the metal hafnium used The purity is 99.92%;

[0026] (2) Put the hafnium tetrafluoride solution into a polytetrafluoroethylene container and put it into a drying box to evaporate to dryness. The temperature of the drying box is 60°C.

[0027] (3) The hafnium tetrafluoride obtained in step (2) is placed in a quartz tube and dehydrated under vacuum and high temperature conditions to obtain solid hafnium tetrafluoride. During vacuum dehydration, add ammonium bifluoride to a polytetrafluoroethylene container filled with hafnium tetrafluoride, and set the vacuum to 16Pa, gradually increase the temperature to 180℃, keep this temperature for 3 hours, and then cool to obtain powdery tetrafluoroethylene Hafnium.

[002...

Embodiment 3

[0031] The method and steps used in Example 2 are the same, except that the excess of hydrofluoric acid is 3%, the temperature of the drying box is 65°C, the vacuum degree of vacuum dehydration is 14Pa, and the temperature is gradually increased to 200°C and kept at this temperature for 4 hours. Cooling is performed to obtain powdered hafnium tetrafluoride.

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PUM

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Abstract

The invention belongs to the field of fluoride preparation technology, and discloses a preparation technology of hafnium tetrafluoride. The preparation technology comprises the following steps of: (1) putting metal hafnium into hydrofluoric acid to obtain hafnium tetrafluoride solution; (2) putting the obtained hafnium tetrafluoride solution into a polytetrafluoroethylene container, and drying by distillation; and (3) putting the hafnium tetrafluoride obtained in the step (2) into a quartz tube, and carrying out dehydration under the conditions of vacuum and high temperature to obtain the solid hafnium tetrafluoride. The preparation technology has the advantages of being simple in operation, and low in oxygen content of the hafnium tetrafluoride.

Description

Technical field [0001] The invention belongs to the technical field of fluoride preparation, and specifically relates to a preparation process of hafnium tetrafluoride. Background technique [0002] 182 Hf is a long-lived nuclide that can provide relevant information about the formation of the moon and the earth, and is widely used to study nuclear astrophysics such as supernovae. In addition, 182 Hf is also a neutron flux monitoring agent, and the measurement of its related physicochemical constants can study the mobility of long-lived radionuclides, which is of great significance to the research on the safe disposal of nuclear waste. But in regular samples 182 The content of Hf is very low, and it is difficult to measure it with general methods. Accelerator mass spectrometry (AMS) has many advantages such as high measurement sensitivity, small sample amount, and short measurement time. 182 An effective method for high sensitivity measurement of Hf. Use AMS to 182 Hf is measure...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G27/04
Inventor 张生栋杨磊孙宏清凡金龙
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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