CN202358933U - Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride - Google Patents
Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride Download PDFInfo
- Publication number
- CN202358933U CN202358933U CN2011202476654U CN201120247665U CN202358933U CN 202358933 U CN202358933 U CN 202358933U CN 2011202476654 U CN2011202476654 U CN 2011202476654U CN 201120247665 U CN201120247665 U CN 201120247665U CN 202358933 U CN202358933 U CN 202358933U
- Authority
- CN
- China
- Prior art keywords
- pipeline
- bottle
- germanium tetrachloride
- tail gas
- vacuum pump
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn - After Issue
Links
Images
Landscapes
- Silicon Compounds (AREA)
Abstract
The utility model discloses a method and an apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride. The characteristics are that a pipeline I is provided on the top of a rectification column on the upper part of a rectifying still, one end of a pipeline II and a tail gas absorbing device are in an inner connection while one other end of the pipeline II is connected with a cooling system and an electromagnet YA1, the pipeline I is in order connected with the cooling system, a discharging electromagnetic pendulum head, a transition bottle, a bubbling bottle, a buffering bottle A, a buffering bottle B, a buffering bottle C, a buffering bottle D and a vacuum pump M, and one other end of the vacuum pump M is communicated with the tail gas absorbing device; that one other tail gas outlet of the transition bottle is in order connected with a liquid level bottle and the tail gas absorbing device through pipelines; that discharging electromagnetic pendulum head is communicated with a waste bottle, a sample tap and a product tank respectively through the pipeline I. The apparatus is advantageous in simple process and convenient operation, and has high value in industrial application for removing hydrogen-containing impurities contained in germanium tetrachloride.
Description
Technical field
The utility model relates to a kind of purifying plant of high purity germanium tetrachloride for optical fibre.Belong to the dissipated metal field of metallurgy.
Background technology
High-purity germanium tetrachloride product is that the high grade quartz of production is the indispensable critical materials of optical fiber, and its purposes is to improve the RI of optical fiber, reduces optical loss, and then improves the transmission range of optical fiber.Because the metal of high-purity germanium tetrachloride and hydrogen containing foreign content are determining the important performance indexes of optical fiber with distributing, its quality directly affects the quality of optical fiber.Therefore, extremely low to the metallic impurity in high-purity germanium tetrachloride (Fe, Co, Cr, Mn, Cu etc.) and the content requirement of hydrogen containing foreign (OH, CH, HCl).
High-purity germanium tetrachloride rectification process of widespread use at present though can remove metallic impurity (Fe, Co, Cr, Mn, Cu etc.) preferably, can't be removed hydrogen containing foreign (OH, CH, HCl) effectively; Even adopt hydrogen chloride gas or anhydrous chlorine to come purifying germanium tetrachloride separately, also can only remove arsenic and other similar impurity, and can not hydrogen containing foreign be removed.
Summary of the invention
The purpose of the utility model is the deficiency that exists to prior art, proposes a kind of device that can effectively remove hydrogen containing foreign in the germanium tetrachloride (OH, CH and HCl), is met the germanium tetrachloride for optical fibre product of optical fiber production.
The technical scheme of the utility model is: a kind of device of removing hydrogen containing foreign in the germanium tetrachloride; It is characterized in that root pipeline I (I) being arranged at the rectifying tower king-post top on rectifying still (3) top; Pipeline II one end connects with device for absorbing tail gas (1) is interior; The pipeline II the other end connects with cooling system (10) and electro-magnet (YA1); With after cooling system (10), discharging electromagnetism yaw (4), transition bottle (5), bubbler (6), surge flask A (11), surge flask B (12), surge flask C (13), surge flask D (14) and vacuum pump (M) connect, vacuum pump (M) the other end connects connection with device for absorbing tail gas (1) to pipeline I (I) more successively; Another tail gas outlet of transition bottle (5) connects with liquid level bottle (7) and device for absorbing tail gas (1) through pipeline III in regular turn;
Discharging electromagnetism yaw (4) is connected with waste material bottle (8), thief hole (9) and product jar (2) respectively through pipeline I (I).
The utility model rectifying tower uses rectifying still to be the common rectifying tower that uses in the industry.
Its step:
(1) is that the germanium tetrachloride of 4N～5N joins in the rectifying still (3) with purity, rectifying still (3) is warming up to carries out rectifying between 75～83 ℃, make germanium tetrachloride be in inferior boiling state; Feeding flow is 30～40L/h nitrogen; Start vacuum pump (M), open valve (YV201e, YV201f, YV201c, YV201b, YV201a and YV201d) simultaneously successively, the pumped vacuum systems operation; Make hydrogen containing foreign pass through pipeline (I) and get into device for absorbing tail gas (1), the pumpdown time is 6--10 hour;
(2) accomplish vacuumize operation process after, continue rising rectifying still temperature, when treating that all sieve plates all present boiling phenomenon in the rectifying tower king-post on rectifying still (3) top, pick up counting and carry out the total reflux operation, the total reflux time is 3--6h;
(3) treat that the total reflux operation process finishes after, open electro-magnet (YA1 and YA2) simultaneously, the adjustment reflux ratio; Control of reflux ratio time 6-8 hour, was adjusted to thief hole (9) one sides with three-way solenoid valve valve (YV202) between 8: 1～12: 1; To the product detection of taking a sample; Such as detection germanium tetrachloride product conform to quality requirements, then three-way solenoid valve valve (YV202) is adjusted to germanium tetrachloride product jar (2) one sides, qualified germanium tetrachloride product changes canned operation over to.
Said reflux ratio is meant: reflux ratio generally is meant the ratio of dirty amount of liquid and rising vapor volume in the tower, and it is called liquid-gas ratio again.Reflux ratio is that cat head cooling dirty process electromagnetism yaw (YA1, YA2) is to rectifying still (3) interior germanium tetrachloride and the ratio that distillates the germanium tetrachloride that produces Bottle & Can (2) in this patent.
Said pumped vacuum systems operation steps is following:
(1) with pipeline (I) successively with after discharging electromagnetism yaw (4), transition bottle (5), bubbler (6), surge flask (11), surge flask (12), surge flask (13), surge flask (14) and vacuum pump (M) connect, vacuum pump (M) goes out the other end and connects with device for absorbing tail gas; Another tail gas outlet of transition bottle (5) connects with liquid level bottle (7) and device for absorbing tail gas (1) through pipeline in regular turn;
(2) rectifying still (3) is warming up between 75～83 ℃, makes germanium tetrachloride be in inferior boiling state;
(3) feeding flow is 30～40L/h high pure nitrogen; Start vacuum pump (M); Open valve YV201e, YV201f, YV201c, YV201b, YV201a and YV201d successively, the operation pumped vacuum systems is observed the liquid level change of liquid level bottle (7) and the variation of system vacuum degree thereof simultaneously;
(4) regulate spinner-type flowmeter (FI17) and vacuum pump (M) pressure regulator valve, make the liquid level difference of liquid level bottle (7) remain on 20-30cm;
(5) along with adding the rising of pining for temperature, observe the change of state of gas-liquid in the rectifying tower, through regulating nitrogen spinner-type flowmeter (FI17), the vacuum tightness and the nitrogen flow of in good time Adjustment System;
(6) when germanium tetrachloride for optical fibre preparation end; Elder generation's valve-off (YV202); After close the rectifying tower heating system, strengthen in the nitrogen flow system and charge into nitrogen, germanium tetrachloride residual in the pipeline is blown into device for absorbing tail gas; Valve-off (YV201d, YV201a, YV201b, YV201c, YV201f, YV201e) is successively closed vacuum pump (M) at last then.
Said nitrogen is the high pure nitrogen of purity 5N--6N.
Principle of work: germanium tetrachloride is liquid under normal temperature, normal pressure, and easily volatilization has very strong corrodibility, is exposed in the air, promptly absorbs airborne moisture content and chemical reaction takes place, and is different according to the mole number of water, and reaction as follows takes place:
Total system must constantly feed high pure nitrogen thus, pollutes germanium tetrachloride to avoid the air admission system.
According to the achievement in research of HANS, HCl is dissolved in GeCl
4Maximum x in the solution can reach x (HCl)=0.028, satisfies Henry's law: x (HCl)=Cp (HCl) log
10(CPa)=-8.270+439 (K/T), rising GeCl
4Solution temperature can reduce the wherein content of the dissolved HCl of institute, when the amount of HCl is reduced to a certain degree; Gas-liquid reaches balance, at this moment, if can destroy this equilibrium state; Constantly reduce the HCl content in the gas phase; HCl in the solution is constantly separated out, and broken belt is not walked, and finally reaches the purpose of removing HCl.Therefore, adopt the measure that vacuumizes to realize this purpose.
The utility model has the advantages that: technological process is simple, and is easy to operate, can remove the hydrogen containing foreign in the germanium tetrachloride well, has higher industrial use value.
Description of drawings
Fig. 1 removes the method for hydrogen containing foreign in the germanium tetrachloride and the optical fiber negative pressure system figure in the device for the utility model.
Among the figure: the 1-device for absorbing tail gas; 2-product jar; The 3-rectifying still; 4-discharging electromagnetism yaw; 5-transition bottle; The 6-bubbler; 7-liquid level bottle; 8-waste material bottle; The 9-thief hole; The 10-cooling system; 11-surge flask, 12-surge flask, 13-surge flask, 14-surge flask; The 15-high pure nitrogen; 16-germanium tetrachloride opening for feed; The 17-rectifying tower;
The M-vacuum pump; The I-pipeline; YV201a, YV201b, YV201c, YV201d, YV201e, YV201f-valve; YV202-three-way solenoid valve valve; YA1, YA2-electro-magnet; The FI17-spinner-type flowmeter.
Embodiment
Embodiment 1:
(1) is that the germanium tetrachloride of 4N～5N joins in the quartzy rectifying still with purity, rectifying still is warming up to carries out rectifying between 75～83 ℃, make germanium tetrachloride be in inferior boiling state; Feeding flow is 30～40L/h nitrogen; Start vacuum pump, open valve YV201e, YV201f, YV201c, YV201b, YV201a and YV201d simultaneously successively, the operation pumped vacuum systems; Make hydrogen containing foreign pass through pipeline I and get into device for absorbing tail gas, the pumpdown time is 6--10 hour;
(2) after completion vacuumizes operation process, continue rising rectifying still temperature, when treating that all sieve plates all present boiling phenomenon in the rectifying tower king-post, pick up counting and carry out the total reflux operation, the total reflux time is 3-6h;
(3) treat that the total reflux operation process finishes after, open electro-magnet YA1, YA2 simultaneously, the adjustment reflux ratio; Control of reflux ratio time 6--8 hour, was adjusted to thief hole one side with three-way solenoid valve YV202 between 8: 1～12: 1; To the product detection of taking a sample; Such as detection germanium tetrachloride product conform to quality requirements, then three-way solenoid valve YV202 is adjusted to canned products one side, change qualified germanium tetrachloride product over to canned operation.
Wherein: the used nitrogen of the production technique of germanium tetrachloride for optical fibre is the high pure nitrogen of purity 5N--6N.
(1) is that the germanium tetrachloride of 4N～5N joins in the quartzy rectifying still 3 and carries out rectifying with 20L purity,, makes germanium tetrachloride be in inferior boiling state rectifying still 3 temperature rises to 80 ℃; The feeding flow is the high pure nitrogen of 30L/h, purity 6N; Start vacuum pump M, open valve YV201e, YV201f, YV201c, YV201b, YV201a and YV201d simultaneously successively, the pumped vacuum systems operation; Make hydrogen containing foreign pass through pipeline I and get into device for absorbing tail gas 1, the pumpdown time is 6 hours;
(2) after completion vacuumizes operation process, continue rising rectifying still 3 temperature, when treating that all sieve plates all present boiling phenomenon in rectifying still 3 king-posts, pick up counting and carry out the total reflux operation, the total reflux time is 3h;
(3) after the total reflux operation process finishes, open electro-magnet YA1, YA2 simultaneously, the adjustment reflux ratio; Control of reflux ratio is between 8: 1, and the time is 6 hours, and three-way solenoid valve YV202 is adjusted to thief hole 9 one sides; To the product detection of taking a sample; Such as detection germanium tetrachloride product conform to quality requirements, then three-way solenoid valve YV202 is adjusted to dress product jar 2 one sides, change qualified germanium tetrachloride product over to canned operation.
Embodiment 2:
(1) is that the germanium tetrachloride of 4N～5N joins in the quartzy rectifying still 3 and carries out rectifying with 25L purity,, makes germanium tetrachloride be in inferior boiling state rectifying still 3 temperature rises to 75 ℃; The feeding flow is the high pure nitrogen of 35L/h, purity 5N; Start vacuum pump, open valve YV201e, YV201f, YV201c, YV201b, YV201a and YV201d simultaneously successively, the operation pumped vacuum systems; Make hydrogen containing foreign pass through pipeline I and get into device for absorbing tail gas 1, the pumpdown time is 10 hours;
(2) after completion vacuumizes operation process, continue rising rectifying still temperature, when treating that all sieve plates all present boiling phenomenon in the rectifying tower king-post, pick up counting and carry out the total reflux operation, the total reflux time is 4h;
(3) after the total reflux operation process finishes, open electro-magnet YA1, YA2 simultaneously, the adjustment reflux ratio; Control of reflux ratio is between 10: 1, and the time is 7 hours, and three-way solenoid valve YV202 is adjusted to thief hole one side; To the product detection of taking a sample; Such as detection germanium tetrachloride product conform to quality requirements, then three-way solenoid valve YV202 is adjusted to canned products one side, change qualified germanium tetrachloride product over to canned operation.
Embodiment 3:
(1) is that the germanium tetrachloride of 4N～5N joins and carries out rectifying in the quartzy rectifying still with 30L purity,, makes germanium tetrachloride be in inferior boiling state still temperature rise to 83 ℃; The feeding flow is the high pure nitrogen of 40L/h, purity 5.5N; Start vacuum pump, open valve YV201e, YV201f, YV201c, YV201b, YV201a and YV201d simultaneously successively, the operation pumped vacuum systems; Make hydrogen containing foreign pass through pipeline I and get into device for absorbing tail gas, the pumpdown time is 10 hours;
(2) after completion vacuumizes operation process, continue rising rectifying still temperature, when treating that all sieve plates all present boiling phenomenon in the rectifying tower king-post, pick up counting and carry out the total reflux operation, the total reflux time is 5h;
(3) after the total reflux operation process finishes, open electro-magnet YA1, YA2 simultaneously, the adjustment reflux ratio; Control of reflux ratio is between 12: 1, and the time is 8 hours, and three-way solenoid valve YV202 is adjusted to thief hole one side; To the product detection of taking a sample; Such as detection germanium tetrachloride product conform to quality requirements, then three-way solenoid valve YV202 is adjusted to product jar one side, change qualified germanium tetrachloride product over to canned operation.
Hydrogen containing foreign transmitance (%) sees the following form in the germanium tetrachloride that original technology and the utility model are obtained:
Can find out from last table, adopt this to invent said method and all can obtain the germanium tetrachloride of hydrogen containing foreign transmitance more than 95%, and the reflux ratio that is adopted be high more, can obtain the higher product of hydrogen containing foreign transmitance.
Claims (1)
1. device of removing hydrogen containing foreign in the germanium tetrachloride; It is characterized in that root pipeline I (I) being arranged at the rectifying tower king-post top on rectifying still (3) top; Pipeline II one end connects with device for absorbing tail gas (1) is interior; The pipeline II the other end connects with cooling system (10) and electro-magnet (YA1); With after cooling system (10), discharging electromagnetism yaw (4), transition bottle (5), bubbler (6), surge flask A (11), surge flask B (12), surge flask C (13), surge flask D (14) and vacuum pump (M) connect, vacuum pump (M) the other end connects connection with device for absorbing tail gas (1) to pipeline I (I) more successively; Another tail gas outlet of transition bottle (5) connects with liquid level bottle (7) and device for absorbing tail gas (1) through pipeline III in regular turn;
Discharging electromagnetism yaw (4) is connected with waste material bottle (8), thief hole (9) and product jar (2) respectively through pipeline I (I).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202476654U CN202358933U (en) | 2011-07-13 | 2011-07-13 | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202476654U CN202358933U (en) | 2011-07-13 | 2011-07-13 | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202358933U true CN202358933U (en) | 2012-08-01 |
Family
ID=46570137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202476654U Withdrawn - After Issue CN202358933U (en) | 2011-07-13 | 2011-07-13 | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202358933U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328951A (en) * | 2011-07-13 | 2012-01-25 | 云南驰宏锌锗股份有限公司 | Method and device for removing hydrogen-containing impurities from germanium tetrachloride |
| CN104236973A (en) * | 2014-09-05 | 2014-12-24 | 武汉云晶飞光纤材料有限公司 | Pre-treatment and sampling device and method for detecting industrial germanium tetrachloride |
-
2011
- 2011-07-13 CN CN2011202476654U patent/CN202358933U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102328951A (en) * | 2011-07-13 | 2012-01-25 | 云南驰宏锌锗股份有限公司 | Method and device for removing hydrogen-containing impurities from 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 |
| CN104236973A (en) * | 2014-09-05 | 2014-12-24 | 武汉云晶飞光纤材料有限公司 | Pre-treatment and sampling device and method for detecting industrial germanium tetrachloride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102328951B (en) | Method and device for removing hydrogen-containing impurities from germanium tetrachloride | |
| CN104925759B (en) | Continuous production method of sulfuric acid with ultrahigh purity | |
| CN202358933U (en) | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride | |
| CN201473330U (en) | Production system for super-high purity aqueous ammonia | |
| CN101871573A (en) | Liquid chlorine vaporization device | |
| CN103566606B (en) | Multifunctional purification device and method for purifying ammonium bifluoride by using same | |
| CN102502701B (en) | Production process and preparation method of ultrapure ammonia | |
| CN110745830A (en) | Method and system for controlling balance of dichlorosilane in polycrystalline silicon production | |
| CN103407971B (en) | Novel technology for production of liquid sulfur dioxide | |
| CN101343040B (en) | Liquefied chlorine flash evaporation purification preparation technique | |
| CN201333371Y (en) | High pressure gas purifier and high pressure gas purification device | |
| CN208948863U (en) | A kind of high-purity ammon continuous process system | |
| CN109231238B (en) | High-purity ammonia continuous production system and production process thereof | |
| CN103159230A (en) | Preparation method of high-purity ammonia water | |
| CN202157120U (en) | Numerical-control intelligent double-water internal cooling oxyhydrogen generator | |
| CN209940473U (en) | Phosphorus trichloride's refining equipment | |
| CN204824176U (en) | Pure phosphorous oxychloride's of 5N level superelevation continuous purification system | |
| CN202729802U (en) | Production device of electronic-grade phosphoric acid | |
| CN104261412A (en) | Method and system for treating crude trichlorosilane | |
| CN206773421U (en) | One kind hydrogenation purification system closed loop Automatic-hydrogenation control system | |
| CN208500356U (en) | A kind of device purifying high-purity argon gas | |
| CN214597413U (en) | Zinc chloride methanol solution solid-liquid separation system | |
| CN213834566U (en) | Novel ammonia purification device | |
| CN101417801B (en) | Conveying method of high temperature liquid chlorosilane | |
| CN218740249U (en) | Cryogenic tail gas material removing device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20120801 Effective date of abandoning: 20140806 |
|
| RGAV | Abandon patent right to avoid regrant |