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Production technology of optical fiber grade high purity ger manium tetrachloride

A pure germanium tetrachloride, production process technology, applied in the field of purification of high-purity compounds, can solve problems such as unreachable effects, achieve the effect of simple process and avoid solution transfer

Inactive Publication Date: 2005-03-23
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another U.S. Patent 6,110,258 reported that zeolite was used to remove water molecules in gases (including germanium tetrachloride gas), but the effect could not reach the level of 6N

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the production technique of fiber-grade high-purity germanium tetrachloride of the present invention comprises the following steps:

[0018] l. Heating the whole set of equipment, heating all parts with a hair dryer and vacuuming, after reaching the ultimate vacuum, pumping for a period of time, and then flushing nitrogen to atmospheric pressure; repeat a total of three times.

[0019] 2. Under a nitrogen protective atmosphere, add about 50 grams of anhydrous calcium chloride and about 500 grams of crude germanium tetrachloride.

[0020] 3. Heat the crude germanium tetrachloride to 80°C, inject hydrogen chloride and chlorine gas, illuminate with an iodine-tungsten lamp, and reflux for 4 hours.

[0021] 4. Heat the quartz tube at 400°C.

[0022] 5. The fractionation column is kept warm for distillation, and the condensate is low-temperature brine.

[0023] 6. Take about 30ml of the previous fraction and obtain about 150ml of the middle fraction.

[0024]...

Embodiment 2

[0026] Embodiment 2: the production technique of fiber grade high-purity germanium tetrachloride of the present invention, its step is:

[0027] 1. Heating the whole set of equipment, heating all parts with a hair dryer and vacuuming, after reaching the ultimate vacuum, pumping for a period of time, then flushing nitrogen to atmospheric pressure, repeating a total of three times.

[0028] 2. Under an argon protective atmosphere, add about 50 grams of non-oxidized phosphorus and about 1000 grams of crude germanium tetrachloride.

[0029] 3. Heat the crude germanium tetrachloride to 60°C, inject hydrogen chloride and chlorine gas, illuminate with a bromine tungsten lamp, and reflux for 6 hours.

[0030] 4. Heating the quartz tube at a temperature of 600°C.

[0031] 5. Insulate the fractionation column for distillation, and the condensate is tap water.

[0032] 6. Take about 50ml of the previous fraction and obtain about 400ml of the middle fraction.

[0033] 7. Under argon pr...

Embodiment 3

[0035] Embodiment 3: the production technique of fiber grade high-purity germanium tetrachloride of the present invention, its step is:

[0036] 1. Heat the whole set of equipment, heat each part with a hair dryer and vacuumize it. After reaching the ultimate vacuum, pump it for a period of time, and then inject nitrogen gas to atmospheric pressure; repeat a total of three times.

[0037] 2. Under nitrogen protection atmosphere, add about 10 grams of magnesium compound and about 1000 grams of crude germanium tetrachloride.

[0038] 3. Heat the crude germanium tetrachloride to 90°C, feed hydrogen chloride and chlorine gas, use a photoinitiator, and reflux for 2 hours.

[0039] 4. Heat the quartz tube at a temperature of 300°C.

[0040] 5. The fractionation column is kept warm for distillation, and the condensate is low-temperature brine.

[0041] 6. Take about 50ml of the previous fraction and obtain about 400ml of the middle fraction.

[0042] 7. Under nitrogen protection, ...

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PUM

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Abstract

A process for preparing the optical fibre-class high-purity GeCl4 includes such steps as making the rectifying apparatus in non-oxygen and non-water state, proportionally adding catalyst and coarse GeCl4 under protection of inertial gas, introducing halide gas, light triggered reflux and distilling, and transferring product under protection of inertial gas.

Description

1. Technical field [0001] The invention relates to a method for purifying high-purity compounds, in particular to a method for purifying high-purity germanium tetrachloride used in optical fiber production. 2. Background technology [0002] Optical fiber is the foundation of optical communication technology and industry. High-purity germanium tetrachloride is an indispensable key raw material for high-grade quartz optical fiber. Germanium tetrachloride is the main dopant in quartz optical fiber. Its purpose is to improve the refraction of optical fiber. Index, reduce optical loss, and then increase the transmission distance of the optical fiber. The distribution and content of germanium in the optical fiber determine the key performance indicators of the optical fiber, so its quality directly affects the performance and quality of the optical fiber. [0003] According to German patent DE-AS No.1263730 report, germanium tetrachloride can be purified by hydrogen chloride. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
Inventor 潘毅赵蕾吕宝源曹季
Owner NANJING UNIV
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