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Method and device for removing hydrogen-containing impurities from germanium tetrachloride

A germanium tetrachloride and impurity technology, applied in the direction of germanium halide, etc., can solve the problems of inability to effectively remove hydrogen-containing impurities and hydrogen-containing impurities, and achieve high industrial use value, convenient operation, and simple process.

Active Publication Date: 2012-01-25
云南驰宏国际锗业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The currently widely used high-purity germanium tetrachloride rectification process can remove metal impurities (Fe, Co, Cr, Mn, Cu, etc.) well, but cannot effectively remove hydrogen-containing impurities (OH, CH, HCl) ; Even if hydrogen chloride gas or anhydrous chlorine gas is used alone to purify germanium tetrachloride, arsenic and other similar impurities can only be removed, but hydrogen-containing impurities cannot be removed

Method used

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  • Method and device for removing hydrogen-containing impurities from germanium tetrachloride

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Experimental program
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Effect test

Embodiment 1

[0030] (1) Add germanium tetrachloride with a purity of 4N to 5N into the quartz rectification kettle, heat the rectification kettle to 75-83°C for rectification, make the germanium tetrachloride in a sub-boiling state, and feed The flow rate is 30-40L / h nitrogen, start the vacuum pump, and at the same time open the valves YV201e, YV201f, YV201c, YV201b, YV201a and YV201d in sequence, and run the vacuum system to make the hydrogen-containing impurities enter the exhaust gas absorption device through the pipeline I. The vacuum time is 6--10 hours;

[0031] (2) After completing the vacuuming operation process, continue to increase the temperature of the rectification kettle, and when all the sieve plates in the column of the rectification tower are boiling, start timing to perform the full reflux operation, and the total reflux time is 3-6h;

[0032] (3) After the full reflux process is over, turn on the electromagnets YA1 and YA2 at the same time, adjust the reflux ratio, and c...

Embodiment 2

[0038](1) 25L of germanium tetrachloride with a purity of 4N to 5N is added to the quartz rectification kettle 3 for rectification, and the temperature of the rectification kettle 3 is raised to 75° C. For high-purity nitrogen gas with a flow rate of 35L / h and a purity of 5N, start the vacuum pump, and at the same time open the valves YV201e, YV201f, YV201c, YV201b, YV201a and YV201d in sequence, and operate the vacuum system to allow hydrogen-containing impurities to enter the tail gas absorption device 1 through the pipeline I , the vacuuming time is 10 hours;

[0039] (2) After completing the vacuuming operation process, continue to increase the temperature of the rectification kettle, and when all the sieve plates in the column of the rectification tower are boiling, start timing and perform the total reflux operation, and the total reflux time is 4 hours;

[0040] (3) After the full reflux process is over, turn on the electromagnets YA1 and YA2 at the same time to adjust ...

Embodiment 3

[0042] (1) Add 30L of germanium tetrachloride with a purity of 4N to 5N into a quartz rectification kettle for rectification, raise the temperature of the kettle to 83°C, make the germanium tetrachloride in a sub-boiling state, and feed in a flow rate of 40L / h. High-purity nitrogen with a purity of 5.5N, start the vacuum pump, and at the same time open the valves YV201e, YV201f, YV201c, YV201b, YV201a and YV201d in sequence, and run the vacuum system to make the hydrogen-containing impurities enter the exhaust gas absorption device through the pipeline I. for 10 hours;

[0043] (2) After completing the vacuuming operation process, continue to increase the temperature of the rectification kettle, and when all the sieve plates in the column of the rectification tower are boiling, start timing and perform the total reflux operation, and the total reflux time is 5 hours;

[0044] (3) After the full reflux process is over, turn on the electromagnets YA1 and YA2 at the same time to...

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Abstract

The invention discloses a method and a device for removing hydrogen-containing impurities from germanium tetrachloride. The method comprises the steps of: using rectified germanium tetrachloride as raw materials, adding germanium tetrachloride with the purity being 4N-5N into a rectifying kettle for rectification, increasing the temperature of the kettle to 75-83 DEG C for rectification, keeping the germanium tetrachloride to be in a sub-boiling state and feeding in nitrogen with the flow rate being 30-40L / h to exhaust HCl gas, wherein exhaust time is no less than 6 hours; after the HCl gas is exhausted, continuously increasing the temperature of the kettle, and when all sieve plates of a rectifying column are in a boiling state, starting to calculate total reflux time, wherein the total reflux time is no less than 3 hours; and after total reflux is completed, turning on a switch of an electromagnetic valve to adjust the reflux ratio to be 8:1 to 12:1, taking products at a front section, detecting the distilled germanium tetrachloride, if the detected products satisfy the production requirement of the germanium tetrachloride for optical fibers, putting the electromagnetic valve on the side with the products being taken, and finally shifting to a filling process after the obtained germanium tetrachloride products are detected as acceptable. The method and the device for removing the hydrogen-containing impurities from the germanium tetrachloride have the advantages that the technological process is simple, the operation is simple, the hydrogen-containing impurities can be well removed from the germanium tetrachloride, and the industrial use value is very high.

Description

technical field [0001] The invention relates to a method and a device for purifying germanium tetrachloride for high-purity optical fibers. It belongs to the field of rare metal metallurgy. Background technique [0002] High-purity germanium tetrachloride is an indispensable key raw material for the production of high-grade quartz-based optical fibers. Its purpose is to increase the refractive index of the optical fiber, reduce optical loss, and increase the transmission distance of the optical fiber. Because the content and distribution of metal and hydrogen-containing impurities in high-purity germanium tetrachloride determine the important performance indicators of the optical fiber, its quality directly affects the quality of the optical fiber. Therefore, the requirements for the content of metal impurities (Fe, Co, Cr, Mn, Cu, etc.) and hydrogen-containing impurities (OH, CH, HCl) in high-purity germanium tetrachloride are extremely low. [0003] The currently widely ...

Claims

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Application Information

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IPC IPC(8): C01G17/04
Inventor 王少龙周廷熙王瑞山匡子登何斌方锦侯明
Owner 云南驰宏国际锗业有限公司
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