Preparation purification method of germanium tetrachloride for optical fiber

A technology of germanium tetrachloride and a purification method, applied in the chemical industry, can solve the problems of low production efficiency, reduction of the total amount of GeCl4, etc., and achieve the effects of high production efficiency, easy process and stable process conditions

Inactive Publication Date: 2013-07-03
GRINM ELECTRO OPTIC MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method uses high-concentration lye, a small amount of GeCl4 will still be hydrolyzed to generate GeO2, which will reduce the total amount of GeCl4 and lower production efficiency.

Method used

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  • Preparation purification method of germanium tetrachloride for optical fiber
  • Preparation purification method of germanium tetrachloride for optical fiber
  • Preparation purification method of germanium tetrachloride for optical fiber

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Experimental program
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Embodiment Construction

[0024] 1. Chlorination distillation:

[0025] In a 500L acid-resistant enamel distillation kettle, first add 35Kg of ferric chloride, then add 60Kg of germanium concentrate, close the solid feed port, add 400L HCl and 15L H 2 SO 4 . Set the kettle temperature of the chlorination enamel kettle at 60-120°C, energize and heat up and stir. When there is no more GeCl in the feed pipe 4 When flowing out, stop the distillation. See the diagram of the chlorination reaction device figure 1 .

[0026] 2. Double steam distillation:

[0027] Add 25L of analytically pure hydrochloric acid to the 50L primary double-steaming reactor, add 800g of manganese dioxide, then add 18L of germanium tetrachloride, add 25L of concentrated hydrochloric acid to the 50L double-steaming reactor, add 500g of manganese dioxide, Open the feed valve of the double steaming once to increase the temperature. And the heating temperature setting range is 60-150℃, and the kettle temperature is controlled at 30-110℃. W...

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Abstract

The invention provides a preparation purification method of germanium tetrachloride for optical fibers, which adopts germanium concentrate as a raw material; hydrochloric acid, sulfuric acid, and ferric trichloride are added into a chlorination reaction vessel according to a certain proportion for reaction to prepare crude germanium tetrachloride; the crude germanium tetrachloride is fully mixed with hydrochloric acid and manganese dioxide according to a certain proportion in a repeated distillation reaction vessel for distillation and purification to obtain preliminarily purified germanium tetrachloride; the germanium tetrachloride after repeated distillation purification is processed in a quartz rectifying tower in inert atmosphere by controlling a tower bottom temperature to be 75-95 DEG C, a tower column temperature to be 30-95 DEG C, and a reflux ratio of 4:1-14:1, so as to obtain high-purity germanium tetrachloride. The high-purity germanium tetrachloride prepared through three procedures of chlorination distillation, repeated distillation, and rectification purification, has a content of transition metal impurities of less than 3 ppb, a content of hydrogen-containing impurities of less than 1 ppm, and meets the requirements for perform rod germanium tetrachloride for optical fibers.

Description

Technical field [0001] The invention belongs to the technical field of chemical engineering, and specifically relates to a preparation and purification method of germanium tetrachloride for optical fiber. Background technique [0002] Optical fiber communication is the most advanced communication technology in the world today. Optical fiber communication has the advantages of large capacity, bandwidth, anti-interference, strong confidentiality and reliability, good stability, low loss, small size, light weight, low cost, and long relay distance. Germanium tetrachloride is one of the key basic materials for the manufacture of communication optical fibers. In the manufacture of optical fibers, germanium tetrachloride is an important dopant in the production of optical fiber preforms. Its function is to increase the refractive index of the fiber core and reduce optical loss. , Thereby increasing the transmission distance of the optical fiber. Therefore, the requirements for the pu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
Inventor 袁琴武鑫萍刘福财莫杰耿宝利
Owner GRINM ELECTRO OPTIC MATERIALS
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