CN101269836B - Rectification column for removing hydrogen containing foreign matter in germanic chloride - Google Patents

Rectification column for removing hydrogen containing foreign matter in germanic chloride Download PDF

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Publication number
CN101269836B
CN101269836B CN2008100583599A CN200810058359A CN101269836B CN 101269836 B CN101269836 B CN 101269836B CN 2008100583599 A CN2008100583599 A CN 2008100583599A CN 200810058359 A CN200810058359 A CN 200810058359A CN 101269836 B CN101269836 B CN 101269836B
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China
Prior art keywords
tower
pipe
head
germanium tetrachloride
hydrogen containing
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CN2008100583599A
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Chinese (zh)
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CN101269836A (en
Inventor
周廷熙
王少龙
钟文
晏勇
彭明清
阎建英
王瑞山
冯玉庭
张文金
张院萍
杨光玉
赵华
汪世银
李恒方
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Yunnan Chihong International Germanium Industry Co ltd
Yunnan Chihong Zinc and Germanium Co Ltd
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Yunnan Chihong Zinc and Germanium Co Ltd
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Priority to CN2008100583599A priority Critical patent/CN101269836B/en
Publication of CN101269836A publication Critical patent/CN101269836A/en
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Abstract

The invention relates to a distillation column eliminating the CH impurity and the HCI impurity in germanium tetrachloride for optical fibers, and the distillation column is mainly used for solving the problem for eliminating the CH impurity and the HCI impurity in the germanium tetrachloride, and the distillation column belongs to the field of special equipment. The distillation column is mainly composed of a column reactor, a column pipe and a column head. The column head is provided with a spiral cooling pipe, a cooling water inlet and a cooling water outlet, and the top of the column head is provided with a gas exit. A pipeline which is linked with a swinging head discharging port is arranged on the gas exit, and the lower part is pumped in the bottom of the column head. The bottom of the swinging head discharging port is provided with the pipeline to be pumped in the upper part of the column pipe, and the column reactor is provided with a feed port, a gas supply port, a temperature monitoring port and a waste discharge port.

Description

A kind of rectifying tower of removing hydrogen containing foreign in the germanium tetrachloride
Technical field
The present invention relates to a kind ofly in producing the germanium tetrachloride for optical fibre product, remove the rectifying tower of hydrogen containing foreign in the germanium tetrachloride, particularly remove the rectifying tower of CH and HCl impurity.Belong to the specific equipment field.
Background technology
Conventional at present rectifying tower can be removed metallic impurity preferably, as Fe, Co, Cr, Mn, Cu etc., but can't remove hydrogen containing foreign (as CH, HCl) effectively.Adopt hydrogen chloride gas or anhydrous chlorine to come purifying germanium tetrachloride separately, can only remove arsenic and other similar impurity, and can not remove hydrogen containing foreign effectively; Though can handle germanium tetrachloride under the high temperature more than 800 ℃ by high temperature service, making hydrogen atom wherein is hydrogenchloride by chlorinated with chlorine, the final removal that realizes hydrogen containing foreign, and this technology is very high to the requirement of equipment, and complicated operation.
Summary of the invention
The object of the present invention is to provide a kind of rectifying tower of removing hydrogen containing foreign in the germanium tetrachloride, it can remove hydrogen containing foreign in the germanium tetrachloride (CH and HCl) efficiently, easily being lower than under 100 ℃ the temperature, to satisfy the needs of producing germanium tetrachloride for optical fibre.
The technical scheme that the present invention removes the rectifying tower of hydrogen containing foreign in the germanium tetrachloride is:
This rectifying tower mainly is made up of the tower still (1) of bottom, the tower head (3) at top and the tower pipe (2) of connection tower still (1) and tower head (3).
Leave opening for feed (4), gas supply mouth (5) and temperature monitoring mouth (6) at tower still (1) top, at tower still (1) middle part actinolyte (7) is arranged, in tower still (1) bottom heating tube (8) and trash discharge mouth (9) are arranged, tower pipe (2) does not have column plate, is a blank pipe.
Tower head (3) is provided with spirrillum water pipe (16), entrance of cooling water (10) and cooling water outlet (11), tower head (3) highest point has tail gas outlet (12), tower head (3) right lower quadrant is connected to fluid collection tube (14), fluid collection tube (14) is communicated with by the surplus liquid return line of tail gas (13) with tail gas outlet (12), and be connected to yaw discharge port (15) in fluid collection tube (14) bottom, the lower left quarter of yaw discharge port (15) flows the upper lateral part that pipe (17) feeds tower pipe (2) once.
Actinolyte (7) is installed on the axis of tower still (1).Whole removal rectifying tower is a hyalosome, all adopts quartz material.
Beneficial effect of the present invention is: can intuitive and convenient ground observe whole Impurity removal process, and carry out being lower than under 100 ℃ of temperature, simple in structure, easy to operate, safe and reliable, impurity removal efficacy is higher.
Description of drawings
Below in conjunction with accompanying drawing of the present invention, further describe its embodiment.
Fig. 1 removes the rectifying tower synoptic diagram of CH and HCl impurity in the germanium tetrachloride for the present invention.
The tower of 1-shown in figure still, 2-tower pipe, 3-tower head, the 4-opening for feed, 5-gas supply mouth, 6-temperature monitoring mouth, the 7-actinolyte, 8-heating tube, 9-trash discharge mouth, the 10-entrance of cooling water, 11-cooling water outlet, the outlet of 12-tail gas, the surplus liquid return line of 13-tail gas, 14-fluid collection tube, 15-yaw discharge port, 16-spirrillum water pipe, the 17-return line
Embodiment
Embodiment: rectifying tower is made of the tower still 1 of bottom, the tower head 3 on top and the middle part tower pipe 2 of connection tower still 1 and tower head 3, is provided with heating tube 8 and actinolyte 7 in tower still 1.Leave opening for feed 4 and gas supply mouth 5 at tower still 1 top, have temperature monitoring mouth 6, have trash discharge mouth 9 in tower still 1 bottom at tower still 1 sidepiece.
Tower head 3 is provided with spirrillum water pipe 16, entrance of cooling water 10 and cooling water outlet 11, tower head 3 highest points have tail gas outlet 12, tower head 3 right lower quadrants are connected to fluid collection tube 14, fluid collection tube 14 and tail gas outlet 12 is communicated with by the surplus liquid return line 13 of tail gas, and be connected to yaw discharge port 15 in fluid collection tube 14 bottoms, the lower left quarter of yaw discharge port 15 flows the upper lateral part that pipe 17 feeds tower pipe 2 once.
Whole rectifying tower is transparent, all adopts quartz material.
During use, the germanium tetrachloride that needs are purified joins in the tower still 1 by opening for feed 4, after heating, process heating tube 8 makes germanium tetrachloride boiling volatilization, the germanium tetrachloride that evaporates rises by tower pipe (2) and arrives the tower head (3) on this rectifying tower top, through spirrillum water pipe (16) condensation, condensed germanium tetrachloride and is collected or is back in the tower still 1 by return line (17) by control yaw discharge port (15) in the surplus liquid return line of tail gas (13) influent collection tube (14).Removal of impurity technological process of the present invention can be in this rectifying tower continuous recirculation, foreign matter content reaches the germanium tetrachloride for optical fibre standard in germanium tetrachloride, carries out formal discharging and collects qualified product from yaw discharge port 15.
Water coolant enters the circulation back from cooling water outlet 11 discharges from the cooling import 10 of spirrillum water pipe (16).
The real-time monitoring of operating temperature and the timely heating tube of adjusting make Heating temperature reach the required requirement of technology in 6 pairs of tower stills 1 of temperature monitoring mouth.
In heat-processed, according to arts demand, can feed shielding gas from tower still 1 gas supply mouth 5, avoid apparatus of the present invention to be secondary polluted being used for removing hydrogen containing foreign process germanium tetrachloride.
In the removal of impurity process, need open 7 pairs of germanium tetrachlorides of actinolyte and carry out illumination.
Surplus liquid after purifying in this rectifying Tata still 1 is discharged this rectifying tower by trash discharge mouth 9.
The present invention is used for germanium tetrachloride for optical fibre production and removes impurity CH and HCl, to satisfy the purity requirement of germanium tetrachloride for optical fibre product.

Claims (5)

1. rectifying tower of removing hydrogen containing foreign in the germanium tetrachloride, it is characterized in that this rectifying tower mainly is made up of the tower head (3) at the tower still (1) of bottom, top and the tower pipe (2) that connects tower still (1) and tower head (3), opening for feed (4), gas supply mouth (5) and temperature monitoring mouth (6) are left in tower still (1) top, at tower still (1) middle part actinolyte (7) is arranged, heating tube (8) and trash discharge mouth (9) are arranged in tower still (1) bottom.
2. the rectifying tower of hydrogen containing foreign in the removal germanium tetrachloride according to claim 1 is characterized in that tower pipe (2) does not have column plate, is a blank pipe.
3. the rectifying tower of hydrogen containing foreign in the removal germanium tetrachloride according to claim 1, it is characterized in that tower head (3) is provided with spirrillum water pipe (16), entrance of cooling water (10) and cooling water outlet (11), tower head (3) highest point has tail gas outlet (12), tower head (3) right lower quadrant is connected to fluid collection tube (14), fluid collection tube (14) is communicated with by the surplus liquid return line of tail gas (13) with tail gas outlet (12), and be connected to yaw discharge port (15) in fluid collection tube (14) bottom, the lower left quarter of yaw discharge port (15) flows the upper lateral part that pipe (17) feeds tower pipe (2) once.
4. the rectifying tower of hydrogen containing foreign in the removal germanium tetrachloride according to claim 1 is characterized in that actinolyte (7) is installed on the axis of tower still (1).
5. the rectifying tower of hydrogen containing foreign in the removal germanium tetrachloride according to claim 1 is characterized in that whole rectifying tower is a hyalosome, all adopts quartz material.
CN2008100583599A 2008-05-07 2008-05-07 Rectification column for removing hydrogen containing foreign matter in germanic chloride Active CN101269836B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2008100583599A CN101269836B (en) 2008-05-07 2008-05-07 Rectification column for removing hydrogen containing foreign matter in germanic chloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2008100583599A CN101269836B (en) 2008-05-07 2008-05-07 Rectification column for removing hydrogen containing foreign matter in germanic chloride

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CN101269836A CN101269836A (en) 2008-09-24
CN101269836B true CN101269836B (en) 2011-06-08

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101891243B (en) * 2010-06-10 2012-01-11 南京中锗科技股份有限公司 Novel extraction process method for purifying germanium tetrachloride
CN102328951B (en) * 2011-07-13 2014-08-06 云南驰宏锌锗股份有限公司 Method and device for removing hydrogen-containing impurities from germanium tetrachloride
CN106730964A (en) * 2015-11-25 2017-05-31 衡阳恒荣高纯半导体材料有限公司 A kind of distilling apparatus for producing high-purity germanium tetrachloride

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Addressee: Li Zhongqiang

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Effective date of registration: 20230721

Address after: 655011 The second floor of the office building of Chihong Company in Qujing Economic and Technological Development Zone, Yunnan Province

Patentee after: YUNNAN CHIHONG INTERNATIONAL GERMANIUM INDUSTRY Co.,Ltd.

Patentee after: YUNNAN CHIHONG ZINC & GERMANIUM Co.,Ltd.

Address before: 655011 Qujing economic and Technological Development Zone, Yunnan

Patentee before: YUNNAN CHIHONG ZINC & GERMANIUM Co.,Ltd.