CN102328951A - Method and device for removing hydrogen-containing impurities from germanium tetrachloride - Google Patents
Method and device for removing hydrogen-containing impurities from germanium tetrachloride Download PDFInfo
- Publication number
- CN102328951A CN102328951A CN201110196635A CN201110196635A CN102328951A CN 102328951 A CN102328951 A CN 102328951A CN 201110196635 A CN201110196635 A CN 201110196635A CN 201110196635 A CN201110196635 A CN 201110196635A CN 102328951 A CN102328951 A CN 102328951A
- Authority
- CN
- China
- Prior art keywords
- germanium tetrachloride
- pipeline
- tail gas
- rectifying
- 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.)
- Granted
Links
Images
Landscapes
- Silicon Compounds (AREA)
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
The present invention relates to a kind of method of purification and device 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 objective of the invention is deficiency, propose a kind of technology and the device that can effectively remove hydrogen containing foreign in the germanium tetrachloride (OH, CH and HCl), be met the germanium tetrachloride for optical fibre product of optical fiber production to the prior art existence.
Technical scheme of the present invention is: 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.
A kind of device of removing hydrogen containing foreign in the germanium tetrachloride; It is characterized in that root pipeline (I) being arranged at the rectifying tower king-post top on rectifying still (3) top; Pipeline one end connects with device for absorbing tail gas (1) is interior; The pipeline 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 (11), surge flask (12), surge flask (13), surge flask (14) and vacuum pump (M) connect, vacuum pump (M) the other end connects connection with device for absorbing tail gas (1) to pipeline (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 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).
Rectifying tower of the present invention uses rectifying still to be the common rectifying tower that uses in the industry.
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.
Advantage of the present invention is: 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 present invention.
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 present invention 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 (4)
1. method of removing hydrogen containing foreign in the germanium tetrachloride is characterized in that removing the concrete step of hydrogen containing foreign in the germanium tetrachloride:
(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.
2. the method for hydrogen containing foreign in the removal germanium tetrachloride according to claim 1 is characterized in that 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 (F117), 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.
3. the production technique of germanium tetrachloride for optical fibre according to claim 1 is characterized in that said nitrogen is the high pure nitrogen of purity 5N--6N.
4. device of removing hydrogen containing foreign in the germanium tetrachloride; It is characterized in that root pipeline (I) being arranged at the rectifying tower king-post top on rectifying still (3) top; Pipeline one end connects with device for absorbing tail gas (1) is interior; The pipeline 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 (11), surge flask (12), surge flask (13), surge flask (14) and vacuum pump (M) connect, vacuum pump (M) the other end connects connection with device for absorbing tail gas (1) to pipeline (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 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).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110196635.XA CN102328951B (en) | 2011-07-13 | 2011-07-13 | Method and device for removing hydrogen-containing impurities from germanium tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110196635.XA CN102328951B (en) | 2011-07-13 | 2011-07-13 | Method and device for removing hydrogen-containing impurities from germanium tetrachloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102328951A true CN102328951A (en) | 2012-01-25 |
| CN102328951B CN102328951B (en) | 2014-08-06 |
Family
ID=45480948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110196635.XA Active CN102328951B (en) | 2011-07-13 | 2011-07-13 | Method and device for removing hydrogen-containing impurities from germanium tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102328951B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976395A (en) * | 2012-11-19 | 2013-03-20 | 云南驰宏锌锗股份有限公司 | Production system of germanium tetrachloride for optical fiber |
| CN103754428A (en) * | 2014-01-14 | 2014-04-30 | 武汉云晶飞光纤材料有限公司 | Method for filling germanium tetrachloride for optical fibers |
| CN104164577A (en) * | 2014-07-25 | 2014-11-26 | 武汉云晶飞光纤材料有限公司 | Method for recovering germanium from tail gas generated by distillation of 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 |
| CN104353259A (en) * | 2014-11-04 | 2015-02-18 | 李桂芳 | Combined rectifying column and application thereof |
| 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 |
| CN112546659A (en) * | 2020-12-08 | 2021-03-26 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3329584A (en) * | 1963-08-20 | 1967-07-04 | Sylvania Electric Prod | Purification of germanium tetrachloride with added ammonium hydroxide |
| US4842839A (en) * | 1985-01-25 | 1989-06-27 | U.S. Philips Corporation | Process for the removal of hydrogen from hydrogen compounds dissolved in silicon tetrachloride or germanium tetrachloride |
| CN1597533A (en) * | 2004-07-27 | 2005-03-23 | 南京大学 | Production technology of optical fiber grade high purity ger manium tetrachloride |
| CN1842491A (en) * | 2004-08-04 | 2006-10-04 | 德古萨公司 | Method and device for purifying silicon tetrachloride or germanium tetrachloride containing hydride |
| CN101234780A (en) * | 2008-03-05 | 2008-08-06 | 云南驰宏锌锗股份有限公司 | Method for producing germanium tetrachloride for optical fibre |
| CN101269836A (en) * | 2008-05-07 | 2008-09-24 | 云南驰宏锌锗股份有限公司 | Rectification column for removing hydrogen containing foreign matter in germanic chloride |
| CN101269835A (en) * | 2008-05-07 | 2008-09-24 | 云南驰宏锌锗股份有限公司 | Apparatus for separating hydrochloric acid from germanic chloride for optical fiber |
| CN202358933U (en) * | 2011-07-13 | 2012-08-01 | 云南驰宏锌锗股份有限公司 | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride |
-
2011
- 2011-07-13 CN CN201110196635.XA patent/CN102328951B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3329584A (en) * | 1963-08-20 | 1967-07-04 | Sylvania Electric Prod | Purification of germanium tetrachloride with added ammonium hydroxide |
| US4842839A (en) * | 1985-01-25 | 1989-06-27 | U.S. Philips Corporation | Process for the removal of hydrogen from hydrogen compounds dissolved in silicon tetrachloride or germanium tetrachloride |
| CN1597533A (en) * | 2004-07-27 | 2005-03-23 | 南京大学 | Production technology of optical fiber grade high purity ger manium tetrachloride |
| CN1842491A (en) * | 2004-08-04 | 2006-10-04 | 德古萨公司 | Method and device for purifying silicon tetrachloride or germanium tetrachloride containing hydride |
| US20090020413A1 (en) * | 2004-08-04 | 2009-01-22 | Degussa Gmbh | Process and apparatus for purifying silicon tetrachloride or germanium tetrachloride containing hydrogen compounds |
| CN101234780A (en) * | 2008-03-05 | 2008-08-06 | 云南驰宏锌锗股份有限公司 | Method for producing germanium tetrachloride for optical fibre |
| CN101269836A (en) * | 2008-05-07 | 2008-09-24 | 云南驰宏锌锗股份有限公司 | Rectification column for removing hydrogen containing foreign matter in germanic chloride |
| CN101269835A (en) * | 2008-05-07 | 2008-09-24 | 云南驰宏锌锗股份有限公司 | Apparatus for separating hydrochloric acid from germanic chloride for optical fiber |
| CN202358933U (en) * | 2011-07-13 | 2012-08-01 | 云南驰宏锌锗股份有限公司 | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976395A (en) * | 2012-11-19 | 2013-03-20 | 云南驰宏锌锗股份有限公司 | Production system of germanium tetrachloride for optical fiber |
| CN102976395B (en) * | 2012-11-19 | 2014-09-17 | 云南驰宏锌锗股份有限公司 | Production system of germanium tetrachloride for optical fiber |
| CN103754428A (en) * | 2014-01-14 | 2014-04-30 | 武汉云晶飞光纤材料有限公司 | Method for filling germanium tetrachloride for optical fibers |
| CN104164577A (en) * | 2014-07-25 | 2014-11-26 | 武汉云晶飞光纤材料有限公司 | Method for recovering germanium from tail gas generated by distillation of germanium tetrachloride |
| CN104164577B (en) * | 2014-07-25 | 2015-11-25 | 武汉云晶飞光纤材料有限公司 | A kind of method of Ti recovery from the tail gas that rectifying germanium tetrachloride produces |
| 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 |
| CN104353259A (en) * | 2014-11-04 | 2015-02-18 | 李桂芳 | Combined rectifying column and application thereof |
| CN104353259B (en) * | 2014-11-04 | 2016-04-27 | 李桂芳 | Combined type rectifying column and application thereof |
| 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 |
| CN112546659A (en) * | 2020-12-08 | 2021-03-26 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
| CN112546659B (en) * | 2020-12-08 | 2022-02-15 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102328951B (en) | 2014-08-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102328951A (en) | Method and device for removing hydrogen-containing impurities from germanium tetrachloride | |
| CN102642839A (en) | Processing process of industrial grade silicon tetrachloride | |
| CN202358933U (en) | Apparatus for removing hydrogen-containing impurities contained in germanium tetrachloride | |
| CN1325674C (en) | Metal antimony purifying method and apparatus | |
| CN102963909B (en) | Method for recovering and reutilizing waste ammonia gas in LED (light-emitting diode) manufacturing through ammonia water method | |
| CN105016320A (en) | Continuous refinement system and technology of ultra-pure phosphorus oxychloride of 5N grade | |
| CN111039759A (en) | Preparation method of ultra-clean high-purity isopropanol | |
| CN102502701B (en) | Production process and preparation method of ultrapure ammonia | |
| CN105174233A (en) | Ultra-clean high-purity sulfuric acid production method | |
| CN103407971B (en) | Novel technology for production of liquid sulfur dioxide | |
| CN101343040B (en) | Liquefied chlorine flash evaporation purification preparation technique | |
| CN102963910A (en) | Method for recovering and reutilizing waste ammonia gas in LED (light-emitting diode) manufacturing through compression method | |
| CN101332977A (en) | Method for separating free chlorine in dilute hydrochloric acid | |
| CN104694769B (en) | A kind of production method of clean vanadium liquid | |
| CN205205238U (en) | Water electrolytic hydrogen production denitrogenates device | |
| CN104261412B (en) | Process the method and system of thick trichlorosilane | |
| CN101269836B (en) | Rectification column for removing hydrogen containing foreign matter in germanic chloride | |
| CN104016352A (en) | Method and system for treating polysilicon tail gas | |
| CN204824176U (en) | Pure phosphorous oxychloride's of 5N level superelevation continuous purification system | |
| CN103879977B (en) | A kind of continuous production method of high pure nitric acid and production equipment | |
| CN209940473U (en) | Phosphorus trichloride's refining equipment | |
| CN109231238B (en) | High-purity ammonia continuous production system and production process thereof | |
| CN202157120U (en) | Numerical-control intelligent double-water internal cooling oxyhydrogen generator | |
| CN202729802U (en) | Production device of electronic-grade phosphoric acid | |
| CN101386413B (en) | Method for reducing oxygen and carbon content in metal silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230104 Address after: No. 1, Ningzhou Road, Qujing Economic and Technological Development Zone, Yunnan 655000 Patentee after: YUNNAN CHIHONG INTERNATIONAL GERMANIUM INDUSTRY Co.,Ltd. Address before: 650228 Qujing Economic and Technological Development Zone, Yunnan Province Patentee before: YUNNAN CHIHONG ZINC & GERMANIUM Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230224 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: No. 1, Ningzhou Road, Qujing Economic and Technological Development Zone, Yunnan 655000 Patentee before: YUNNAN CHIHONG INTERNATIONAL GERMANIUM INDUSTRY Co.,Ltd. |