Method for producing germanium tetrachloride for optical fibre

A technology of germanium tetrachloride and a production method, which are applied to the purification of germanium tetrachloride for optical fibers and the purification of high-purity compounds, can solve the problems of high equipment requirements, inability to remove CH impurities, complicated operations and the like, and achieve convenient operation, The effect of high industrial use value and simple process

Inactive Publication Date: 2008-08-06
YUNNAN CHIHONG ZINC & GERMANIUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The currently widely used rectification process can remove metal impurities (Fe, Co, Cr, Mn, Cu, etc.) well, but cannot effectively remove hydrogen-containing impurities (OH, CH, HCl); hydrogen chloride gas alone or anhydrous Chlorine is used to purify germanium tetrachloride, which can only remove arsenic and other similar impurities, but not hydrogen-containing impurities; PCl 3 or PBr 3 Add to SiCl 4 , GeCl 4 and POCl 3 and adding Cl to it 2 or Br 2 , which reacts the -OH group to form HCl (or HBr) and POCl 3 (or POBr 3 ), and then remove HCl and HBr, thereby realizing the removal of OH impurity and HCl impurity in germanium tetrachloride, and this technology cannot remove CH impurity; Atoms are chlorinated into hydrogen chloride by chlorine gas, and finally the removal of hydrogen-containing impurities is achieved, but the process requires very high equipment and complicated operations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) 7L hydrochloric acid and 28L germanium tetrachloride are added to the distillation still and the distillation temperature is 76°C;

[0014] (2) The germanium tetrachloride solution after the distilled solution is separated by the hydrochloric acid separator is stored in a storage tank and needs to be left standing for 36 hours;

[0015] (3) The germanium tetrachloride solution in the storage tank is discharged into the empty tower distillation still, the temperature of the germanium tetrachloride solution is raised to 70° C., and while continuously feeding nitrogen for 12 hours, an ultraviolet lamp is used for illumination, and the ultraviolet light The lamp power is 40W and produces ultraviolet light with a wavelength of 253.7nm. Finally carry out rectification operation and transfer out the product, the rectification temperature is 76 ℃.

Embodiment 2

[0017] (1) 20L of hydrochloric acid and 10L of germanium tetrachloride are added to the distillation kettle for distillation, and the distillation temperature is 80°C;

[0018] (2) The germanium tetrachloride solution after the distilled solution is separated by the hydrochloric acid separator is stored in a storage tank, and needs to be left standstill for 72h;

[0019] (3) The germanium tetrachloride solution in the storage tank is discharged into the empty tower distillation still, the temperature of the germanium tetrachloride solution is raised to 75° C., and while continuously feeding nitrogen for 36 hours, an ultraviolet lamp is used for illumination, and the ultraviolet light The lamp power is 40W and produces ultraviolet light with a wavelength of 253.7nm. Finally carry out rectification operation and transfer out the product, the rectification temperature is 80 ℃.

Embodiment 3

[0021] (1) 10L of hydrochloric acid and 20L of germanium tetrachloride are added to the distillation still, and the distillation temperature is 77°C;

[0022] (2) the germanium tetrachloride solution after the distilled solution is separated in the hydrochloric acid separator is stored in the storage tank, and needs to be left standstill for 48h;

[0023] (3) The germanium tetrachloride solution in the storage tank is discharged into the empty tower distillation still, the temperature of the germanium tetrachloride solution is raised to 72 ° C, and while continuously feeding nitrogen for 18 hours, the ultraviolet lamp is used for illumination, and the ultraviolet light The lamp power is 40W and produces ultraviolet light with a wavelength of 253.7nm. Finally, carry out rectification operation and transfer out the product, the rectification temperature is 77 ℃.

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Abstract

The invention discloses a method for producing germanium tetrachloride for optical fibers, which includes the steps: hydrochloric acid and germanium tetrachloride with a volume ratio of 0.25-2.0: 1 are added into a distiller to be distilled; or while separately distilling the germanium tetrachloride, HCI gas is pumped in until the distilling is finished with the distilling temperature of 76-80 DEG C; after the distilled solution is separated by a hydrochloric separator, the germanium tetrachloride solution is stored in a storage tank to be discharged to an empty tower distiller for 36-72 hours of standing; temperature of the germanium tetrachloride solution is raised to 70-75 DEG C; while continuous pumping nitrogen for 12-36 hours, an ultraviolet lamp is adopted for lighting; finally, distillation operation is carried out at 76-80 DEG C and the product is transferred. The method for producing the germanium tetrachloride for optical fibers has the advantages of simple process course and convenient operation which can remove the impurity containing hydrogen in the germanium tetrachloride with high value for industrial use.

Description

technical field [0001] The invention belongs to the field of rare metal metallurgy, and relates to a method for purifying high-purity compounds, in particular to a method for purifying germanium tetrachloride for optical fiber used in optical fiber production. Background technique [0002] High-purity germanium tetrachloride is an indispensable key raw material for high-grade quartz-based optical fibers. It is used as the main dopant in quartz-based optical fibers. Its purpose is to increase the refractive index of the optical fiber, reduce optical loss, and then increase the transmission distance of the optical fiber. Since the dopant enters the fiber core, its content and distribution determine the important performance indicators of the fiber, and its quality directly affects whether a high-quality fiber can be obtained. Therefore, the requirements for the content of metal impurities (Fe, Co, Cr, Mn, Cu, etc.) and hydrogen-containing impurities (OH, CH, HCl) in germanium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
Inventor 王洪江周廷熙王少龙钟文晏勇彭明清阎建英王瑞山杨光玉赵华何斌赵永波汪世银李恒方李雪寅
Owner YUNNAN CHIHONG ZINC & GERMANIUM
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