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.