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Method and device for preparing high-purity low-metallic impurity tantalum chloride through one-step process

A technology of tantalum pentachloride and low metal, applied in the field of rare metal powder material preparation, can solve the problems of high content of metal impurities and oxychloride, cumbersome process, etc., and achieve the effects of high purity, simple process and short process flow

Active Publication Date: 2017-03-22
湖南省华京粉体材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention develops a one-step method for preparing high-purity and low-metal-impurity tantalum pentachloride for the problems of toxic and harmful waste gas generated in the existing tantalum pentachloride production process, complicated process, and high content of metal impurities and oxychlorides. method and device

Method used

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  • Method and device for preparing high-purity low-metallic impurity tantalum chloride through one-step process
  • Method and device for preparing high-purity low-metallic impurity tantalum chloride through one-step process
  • Method and device for preparing high-purity low-metallic impurity tantalum chloride through one-step process

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Embodiment 1

[0027] The device used in the present invention is as figure 1 As shown, the device consists of four parts: a vertical chlorination furnace 1, a collection tower 2, a vacuum system 3 and a tail gas absorption system 4. Wherein the top of the chlorination furnace 1 is set as a tantalum source feeding port 11, the side bottom is provided with a gas source inlet 13, and the bottom is an ash outlet 14; there is a buffer electric heating belt 15 between the vertical chlorination furnace 1 and the collecting tower 2 , with enough resistance wires to ensure that the temperature of the buffer zone is 300~600°C; the collection tower 2 is composed of an air cooling system 21 at the top 1 / 3 and a water cooling system at the middle 2 / 3, and the bottom of the collection tower 2 is equipped with a finished product A discharge port 23; in addition, a vacuum system 3 is provided at the side of the collection tower near the top 1 / 6, and a tail gas absorption system 4 is provided at the side ne...

Embodiment 2

[0031] Use 1 / 2 tantalum chips and 1 / 2 tantalum powder as the tantalum source, put the tantalum source into the chlorination furnace, control the system vacuum to 0.03Mpa, add inert gas argon with a purity of 99.99%, and react Hydrogen gas with a purity of 99.9% was introduced to hydrogenate the tantalum source, and the hydrogen gas was replaced with inert gas argon for 90 minutes. After the replacement, chlorine gas was introduced to react, and the temperature of the chlorination furnace was controlled at 400°C. The purity of chlorine gas is 99.9%. The molar ratio of tantalum source and chlorine gas is 200:650; the molar ratio of tantalum source:hydrogen gas is 200:200, and the volume of the receiving tower is three times that of the chlorination furnace. The finished tantalum products are analyzed in the following table:

[0032]

Embodiment 3

[0034] Use 1 / 2 tantalum rod and 1 / 2 tantalum block as the tantalum source, put the tantalum source into the chlorination furnace, control the system vacuum to 0.01Mpa, add inert gas argon with a purity of 99.99%, and react The hydrogen gas with a purity of 99.9% was introduced to hydrogenate the tantalum source, and then the hydrogen gas was replaced with an inert gas argon for 120 minutes. After the replacement, chlorine gas was introduced to react, and the temperature of the chlorination furnace was controlled at 400°C. The purity of chlorine gas is 99.9%. The molar ratio of tantalum source and chlorine gas is 200:700; the molar ratio of tantalum source:hydrogen gas is 200:300, and the volume of the receiving tower is 1.5 times that of the chlorination furnace. After 12 hours of reaction, the finished product of tantalum pentachloride is collected and analyzed. As shown in the following table:

[0035]

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Abstract

The invention discloses a method and device for preparing high-purity low-metallic impurity tantalum chloride through a one-step process. Tantalum and chlorine serve as raw materials, wherein the molar ratio is 200:(500-800); before a reaction, nitrogen is injected into a chlorination furnace, wherein the molar ratio of a tantalum source to the nitrogen is 200:(200-300), and injection time is 30-150 minutes; then the nitrogen is replaced with inert gas, preset temperature is reached, chlorine is injected to react for 3-16 hours, and the temperature of the chlorination furnace is 300-600 DEG C. The chlorination furnace is connected with a receiving tower, chlorine / nitrogen / inert gas is injected from the low end of the chlorination furnace, and a vacuum pump is arranged on the side face of the receiving tower. The volume of the receiving tower is 1-5 times that of the chlorination furnace; an air cooling and water cooling combined cooling system is adopted, the tantalum pentachloride is collected from the bottom of the receiving tower, and the metallic impurities of the prepared tantalum pentachloride crystals are 3 ppm or below. The process is short, equipment is simple, energy is saved, environmental friendliness is achieved, a rectifying step is omitted, and the high-purity tantalum pentachloride crystals with the low metallic impurities can be prepared.

Description

technical field [0001] This patent relates to a method and device for preparing high-purity and low-metal-impurity tantalum pentachloride in one step, and belongs to the field of preparation of rare metal powder materials. Background technique [0002] Tantalum pentachloride, white glassy crystal or powder. The relative density is 3.68 (27°C). The melting point is 216°C. The boiling point is 242°C. Soluble in absolute alcohol, sulfuric acid and potassium hydroxide. With the development of modern science and technology, tantalum pentachloride, as a rare metal material, is playing an important role in the field of material chemistry. [0003] The ultra-fine nanometer tantalum powder prepared from tantalum pentachloride is an important raw material for making miniaturized, high specific volume, and high-performance capacitors. At the same time, the tantalum coating synthesized from tantalum pentachloride can greatly increase the corrosion resistance and biocompatibility of...

Claims

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Application Information

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IPC IPC(8): C01G35/02
CPCC01G35/02C01P2006/80Y02P20/10
Inventor 沈季芳戴长欣任改梅李焌源薛海涛李春芳
Owner 湖南省华京粉体材料有限公司
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