Method for producing germanium tetrafluoride

A technology of germanium tetrafluoride and its manufacturing method, which is applied to the preparation of fluorides, germanium halides, etc., and can solve problems such as the control of difficult reactions and the improvement of manufacturing efficiency

Inactive Publication Date: 2011-08-24
CENT GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, when the fluorination reaction of metal germanium is carried out in an open system like the method (d) above, it is difficult to control the reaction and improve the production efficiency.

Method used

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  • Method for producing germanium tetrafluoride
  • Method for producing germanium tetrafluoride
  • Method for producing germanium tetrafluoride

Examples

Experimental program
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Embodiment 1

[0035] 1000 g of metal germanium 3 powder with a purity of 99.99% was filled in the center of a tubular reactor 4 made of nickel with an inner diameter of 80 mm and a length of 1000 mm. The inside of the system was replaced with a vacuum, and the temperature of the outer wall of the reactor 4 was set to 200° C., and helium gas was introduced into the system to make it 80 kPa. The cooling trap 5 was cooled to -60°C. Next, set the circulating flow rate of pump 2 to 6L / min, and pass F 2 Fluorine gas was supplied by a mass flow controller 1 at a flow rate of 400 cc / min, and the reaction was performed for 10 hours. Thereafter, the generated gas trapped in the cooling trap 5 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.) and ultraviolet spectrophotometer (U-2810 manufactured by Hitachi), and it was confirmed that germanium tetrafluoride generate. In addition, the concentration of fluorine gas in the outlet gas of reactor 4 was analyzed using an ultra...

Embodiment 2

[0037] 500 g of metal germanium 3 powder with a purity of 99.99% was filled in the center of a tubular reactor 4 made of nickel with an inner diameter of 80 mm and a length of 1000 mm. Vacuum replacement was performed in the system, and the temperature of the outer wall of the reactor 4 was set at 150° C., and helium gas was introduced into the system to make it 120 kPa. The cooling trap 5 was cooled to -60°C. Next, set the circulating flow rate of pump 2 to 10L / min, and pass F 2 Fluorine gas was supplied at a flow rate of 300 cc / min by a mass flow controller 1, and the reaction was performed for 10 hours. Thereafter, the generated gas trapped in the cooling trap 5 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.) and ultraviolet spectrophotometer (U-2810 manufactured by Hitachi), and it was confirmed that germanium tetrafluoride generate. In addition, the concentration of fluorine gas in the outlet gas of reactor 4 was analyzed using an ultraviol...

Embodiment 3

[0039] 2000 g of metal germanium 3 powder with a purity of 99.99% was filled in the center of a reactor 4 made of nickel with an inner diameter of 130 mm and a length of 700 mm. The inside of the system was replaced with a vacuum, and the temperature of the outer wall of the reactor 4 was set at 250° C., and helium gas was introduced into the system to make it 101 kPa. The cooling trap 5 was cooled to -60°C. Next, set the circulating flow rate of pump 2 to 15L / min, and pass F 2Fluorine gas was supplied at a flow rate of 700 cc / min by a mass flow controller 1, and the reaction was performed for 10 hours. Thereafter, the generated gas trapped in the cooling trap 5 was analyzed by FT-IR (IG-1000 manufactured by Otsuka Electronics Co., Ltd.) and ultraviolet spectrophotometer (U-2810 manufactured by Hitachi), and it was confirmed that germanium tetrafluoride generate. In addition, the concentration of fluorine gas in the outlet gas of reactor 4 was analyzed using an ultraviolet ...

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PUM

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Abstract

A method for producing germanium tetrafluoride, which comprises a step of supplying a fluorine gas into a reactor which is filled with germanium metal and a diluent gas; a step of collecting germanium tetrafluoride, which is a reaction product, by passing the gas discharged from the reactor through a cooling collection unit, and a step of circulating the gas passed through the cooling collection unit back to the reactor. By circulating the gas in the closed system as described above, germanium tetrafluoride can be produced safely and efficiently.

Description

technical field [0001] The invention relates to a method for producing germanium tetrafluoride. Background technique [0002] As a method for producing germanium tetrafluoride, widely known are: (a) a halogen exchange method in which antimony fluoride is reacted with germanium tetrachloride (for example, Non-Patent Document 1); (b) heating germanium hexafluoride Decomposition method (for example, non-patent document 2); (c) method utilizing the reaction of germanium oxide and bromine trifluoride (for example, non-patent document 3); (d) direct fluorination using metal germanium and fluorine gas law etc. [0003] However, germanium tetrafluoride obtained by the methods (a), (b) and (c) above contains germanium fluoride chloride, HF, CO 2 、CF 4 , N 2 , O 2 and other gases. [0004] On the other hand, in the method (d) above, since high-purity metal germanium and fluorine gas can be obtained, high-purity germanium tetrafluoride can be obtained. However, as shown in the f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
CPCC01G17/04C01B9/08C01G1/06
Inventor 梅崎智典毛利勇中原启太
Owner CENT GLASS CO LTD
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