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Method and device for synthesizing and refining optical fiber grade germanium tetrachloride

A technology of germanium tetrachloride and optical fiber, which is applied in the field of synthesis and refining of optical fiber-grade germanium tetrachloride and devices, can solve the problems of increased production cost, high energy consumption of the process, and a large amount of waste acid, so as to save energy consumption and improve The degree of greening and the effect of reducing waste acid

Pending Publication Date: 2020-11-20
TIANJIN ZHONGKE TUOXIN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The addition of concentrated sulfuric acid and concentrated hydrochloric acid requires higher equipment materials, greatly increases production costs, and produces a large amount of waste acid, causing environmental pollution; repeated distillations cause high energy consumption in the process

Method used

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  • Method and device for synthesizing and refining optical fiber grade germanium tetrachloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Attached below figure 1 The present invention will be further described with reference to specific embodiments.

[0060] Add 1000g of germanium powder into the reactor R101, and gradually introduce 2011g of high-purity hydrogen chloride, control the pressure of the reactor to 0.2MPa, the temperature of 200°C, and the reaction time of 8h, the reaction produces 1773g of germanium tetrachloride. The crude germanium tetrachloride (germanium tetrachloride, hydrogen germanium trichloride, hydrogen, hydrogen chloride) obtained through the reaction is collected and dedusted by the cyclone separator CS101 and the bag filter FF101, and then enters the spray tower T201 to remove heavy impurities. The operating pressure of the spray tower T201 is 0.3MPa, and the operating temperature is 123°C. Part of the material at the top of the spray tower T201 is condensed and cooled by the spray tower condenser E201, and part of it returns to the spray tower T201 as spray liquid, and part of...

Embodiment 2

[0063]Add 1000g of germanium powder to the reactor R101, and gradually introduce 4022g of high-purity hydrogen chloride, control the pressure of the reactor to 0.6MPa, the temperature to 300°C, and the reaction time to 4h, the reaction produces 2215.9g of germanium tetrachloride. The crude germanium tetrachloride (germanium tetrachloride, hydrogen germanium trichloride, hydrogen, hydrogen chloride) obtained through the reaction is collected and dedusted by the cyclone separator CS101 and the bag filter FF101, and then enters the spray tower T201 to remove heavy impurities. The operating pressure of the spray tower T201 is 0.1MPa, and the operating temperature is 82°C. Part of the material at the top of the spray tower T201 is condensed and cooled by the spray tower condenser E201, and part of it returns to the spray tower T201 as spray liquid, and part of it enters the light removal tower T301; the uncondensed gas phase is extracted and enters the depth of the dephlegmator E101...

Embodiment 3

[0066] Add 1000g of germanium powder into the reactor R101, and gradually introduce 6033.1g of high-purity hydrogen chloride, control the pressure of the reactor at 1MPa, the temperature of 400°C, and the reaction time of 2h, the reaction produces 2659.1g of germanium tetrachloride. The crude germanium tetrachloride (germanium tetrachloride, hydrogen germanium trichloride, hydrogen, hydrogen chloride) obtained through the reaction is collected and dedusted by the cyclone separator CS101 and the bag filter FF101, and then enters the spray tower T201 to remove heavy impurities. The operating pressure of the spray tower T201 is 0.2MPa, and the operating temperature is 106°C. Part of the material at the top of the spray tower T201 is condensed and cooled by the spray tower condenser E201, and part of it returns to the spray tower T201 as spray liquid, and part of it enters the light removal tower T301; the uncondensed gas phase is extracted and enters the depth of the dephlegmator ...

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Abstract

The invention relates to a method and a device for synthesizing and refining optical fiber grade germanium tetrachloride. The method comprises the steps: making hydrogen chloride and germanium powderreact under the conditions where the pressure is 0.1-1 MPa and the temperature is 200-400 DEG C, wherein the effective conversion rate of germanium is 60-90%, and obtaining germanium tetrachloride crude gas through reaction; removing dust from the germanium tetrachloride crude product and then carrying out heavy component removal treatment, wherein the heavy component removal operation pressure is0.1-0.3 MPa, and the operation temperature is 82-123 DEG C; recovering hydrogen chloride from non-condensable gas generated in the heavy component removal process under the operating condition of -130--80 DEG C, and then discharging the gas; and refining the de-heavy material under the conditions where the pressure is 0.2-0.5 MPa and the temperature is 103-143 DEG C to obtain a 8N optical fiber grade germanium tetrachloride product. Germanium powder and hydrogen chloride are adopted for direct reaction, so that introduction of sulfuric acid and hydrochloric acid is avoided, generation of waste acid and waste salt is reduced, and the greenization degree of the production process is improved. The effective conversion rate of germanium is 80-95%, and compared with a traditional process, energy is saved by more than or equal to 40%.

Description

technical field [0001] The invention relates to a method and device for synthesizing and refining fiber-grade germanium tetrachloride. Background technique [0002] Germanium tetrachloride (GeCl 4 ) is a colorless fuming liquid, commonly used in the production of high-purity germanium dioxide, high-purity germanium and dopants in quartz-based optical fibers. With the development of the modern communication industry, germanium tetrachloride as an optical fiber dopant has the advantages of large transmission capacity, high refractive index, low dispersion, low loss, strong anti-interference ability to nuclear radiation and electromagnetic radiation, and all-weather working ability, etc. Advantages, greatly improving the performance and quality of optical fiber, so that the consumption of germanium in the field of optical fiber manufacturing has increased rapidly. That is, without high-quality germanium tetrachloride, there will be no high-quality silica optical fiber. The t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D3/14B01D3/00C01G17/04
CPCB01D3/009B01D3/14C01G17/04
Inventor 蔡江曾宪友
Owner TIANJIN ZHONGKE TUOXIN TECH CO LTD
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