CN104862500A - Metal germanium recovery device and metal germanium recovery method - Google Patents
Metal germanium recovery device and metal germanium recovery method Download PDFInfo
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- CN104862500A CN104862500A CN201510299886.9A CN201510299886A CN104862500A CN 104862500 A CN104862500 A CN 104862500A CN 201510299886 A CN201510299886 A CN 201510299886A CN 104862500 A CN104862500 A CN 104862500A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a metal germanium recovery device and a metal germanium recovery method, belongs to a metal germanium recovery technology, and relates to a device for recovering metal germanium and a process for secondarily recovering germanium from a waste germanium ingot by virtue of the device. The device comprises a reaction kettle and a heater, wherein a combustion chamber and a condensation chamber are arranged in the reaction kettle; the combustion chamber is heated by the heater, chlorine is introduced, chlorine combustion reaction is performed to directly generate germanium tetrachloride, and germanium tetrachloride is condensed into liquid for collection. According to the device and the method, the whole process is carried out in a quartz container, so that the addition of multiple pieces of equipment such as the reaction kettle is avoided, and production cost is reduced; in addition, the metal germanium recovery process is simple, low in energy consumption and easy to operate, and metal germanium recovery rate is increased, and can reach more than 99 percent.
Description
Technical field
The present invention relates to germanium metal recovery technology, be specifically related to a kind of device of Footwall drift germanium and utilize the processing method of this device secondary recovery germanium from waste and old germanium ingot.
Background technology
Germanium is a kind of important rare metal, and be most important semiconductor material beyond silica removal, germanium system product is widely used in semi-conductor industry, space flight and aviation, and light moves communication, chemical catalyst, the fields such as solar cell.Germanium is scattered in a variety of mineral and rock, but its content is not enough to directly extract from mineral, and therefore the production of germanium comprises germanium concentrate preparation, the extraction of germanium, germanium purification three phases.The source of current germanium is extracted mainly through the pyrometallurgical smelting of germanium brown coal, or from the by product in heavy metal smelting process.Meanwhile, in germanium production process, have a large amount of scrap metal germanium to produce, wherein with monocrystalline germanium ingot, germanium ingot is melted in district, and infrared optics germanium wafer is main.
The method of tradition Footwall drift germanium be mainly be scrap metal germanium is smashed screening levigate after, add excessive sodium hydrate at high temperature roasting and generate sodium germanate, add salt acid distillation and generate germanium tetrachloride gas; Or utilization adds iron trichloride and hydrochloric acid reaction, distillation generates germanium tetrachloride gas, collects germanium tetrachloride liquid after condensation.
China Patent Publication No. CN1465728A discloses a kind of from from the method carrying Ti recovery germanium cinder.The method be by after carrying germanium germanic 0.015% ~ 0.030% cinder, under the furnace temperature of 1150 ~ 1250 DEG C, in stove, cause the weakly reducing atmosphere of CO2 10% ~ 15%, CO 1% ~ 4%, O2 2% ~ 5%, germanium volatilized and is collected in flue dust.But the germanium accumulation rate of the method, cost recovery is high.
China Patent Publication No. CN103334011A discloses a kind of from putting forward germanium cinder and the processing method carrying secondary recovery germanium germanic acid slag.This technique includes washing depickling and dechlorination, broken batching, smelts, collects processing step prepared by germanium concentrate and germanium dioxide, and it is also by hydrochloric acid Distillation recovery.This technique rate of recovery and accumulation rate higher, but complex process.
According to above-mentioned, at present to the recovery process of germanium metal mainly by adding iron trichloride or sodium hydroxide, recycling hydrochloric acid distills out germanium tetrachloride.Complex process, the rate of recovery and accumulation rate low, cost is high.
Summary of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of Footwall drift germanium device, this apparatus design is simple, and concise in technology, easy to operate, cost is low.
The present invention also provides a kind of processing method utilizing Footwall drift germanium device secondary recovery germanium from waste and old germanium ingot, and adopt chlorine combustion method to carry out burning evaporation to germanium metal, technique is simple, and without the need to all genus equipment of overpaying such as steel lining enamel, the rate of recovery is high, and production cost is low.
A kind of Footwall drift germanium device, include reactor, reactor is combustion chamber and condensing chamber by baffle for separating; Dividing plate is provided with production well, and described reactor and separator material are quartz.
Described combustion chamber is provided with inlet mouth and opening for feed, and opening for feed can seal with sealing plug.
Bottom, described combustion chamber is provided with well heater, and described well heater heats combustion chamber, can control heating at any time, safe ready.
Be provided with spiral tube in described condensing chamber, spiral tube one end is connected with production well, and the other end is connected with discharge port; The germanium tetrachloride gas produced in combustion chamber enters spiral tube in condensing chamber by production well, is condensed into liquid and flows out, collected by discharge port.
Described condensing chamber is provided with rising pipe, water inlet pipe and discharge port, be filled with cooling medium at spiral tube space outerpace, and cooling medium is by the flowing of water inlet pipe and rising pipe, carry out condensation to germanium tetrachloride gas in spiral tube, condensed liquid is collected by discharge port.
The present invention also provides a kind of method utilizing Footwall drift germanium device Footwall drift germanium from waste and old germanium ingot, comprise following methods step: loaded by waste and old germanium ingot in the combustion chamber of reactor, utilize well heater by when temperature rises to 400--600 DEG C in combustion chamber, pass into by the chlorine produced after liquid chlorine vaporization, combustion reactions occurs, and germanium tetrachloride gas produce liquid after the cooling medium condensation in condensing chamber of generation is collected.
In described condensing chamber, cooling medium is the salt solution of-8 DEG C, germanium tetrachloride gas rapid condensation can be made to be liquid, collect.
Under described well heater is arranged on combustion chamber, combustion chamber direct heating is heated up, makes burning room temp reach 400--600 DEG C, cause chlorine and the burning of waste and old germanium ingot.
Temperature of combustion in described combustion chamber controls at 400--600 DEG C, produces germanous chloride when temperature of combustion can be prevented too low; Inlet mouth is provided with flow control valve and under meter, and can observe chlorine flowrate and regulate, temperature be controlled by chlorine flowrate, passes into Lv Qi Liu Liang Di large-scale combustion temperature higher, can cause waste when chlorine flowrate is excessive.The considerable production well place looked on the dividing plate of combustion chamber does not have white smoke to produce, and having in combustion chamber during bright blue flame is optimum temps and chlorine flowrate.
Described well heater, when passing into chlorine and carrying out combustion reactions, is cut off the electricity supply, is deactivated.
Described waste and old germanium ingot is without granularity requirements, and in combustion chamber, same section of face piles up more than three pieces simultaneously.
Chemical equation involved in the present invention is as follows:
Ge+2Cl
2＝GeCl
4
Beneficial effect of the present invention is:
The present invention adopts chlorine combustion method directly to carry out burning evaporation to waste and old germanium ingot, then collects after carrying out condensation, and technical process is simple; After utilizing well heater to heat up to the combustion chamber in reactor, deactivate in combustion reactions stage heater, reduce energy consumption; Inlet mouth is provided with flow control valve and under meter, and can regulate chlorine flowrate and observe, and then control at 400--600 DEG C by temperature, improve the rate of recovery of germanium metal, the rate of recovery of germanium metal can reach more than 99%, also avoid the waste of chlorine; Whole process is carried out in a kettle., does not increase many equipment such as steel lining enamel, reduces production cost.
Accompanying drawing explanation
Accompanying drawing 1 is the schematic diagram of a kind of Footwall drift germanium of the present invention device.
1-combustion chamber, 2-condensing chamber, 3-well heater, 4-inlet mouth, 5-opening for feed, 6-sealing plug, 7-production well, 8-dividing plate, 9-spiral tube, 10-water inlet pipe, 11-rising pipe, 12-discharge port, 13-reactor.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing 1 pair of Footwall drift germanium device and utilize this device to carry out germanium metal recovery method further description.
A kind of Footwall drift germanium device, as shown in Figure 1, comprise reactor 13 and well heater 3, wherein reactor 13 is divided into combustion chamber 1 and condensing chamber 2 by dividing plate 8, its median septum 8 is provided with production well 7, and well heater 3 is arranged on bottom, combustion chamber 1, can heat combustion chamber 1, combustion chamber 1 is provided with inlet mouth 4 and opening for feed 5, and opening for feed 5 can seal with sealing plug 6.Spiral tube 9 is provided with in condensing chamber 2, spiral tube 9 one end is connected with production well 7, the other end is connected with discharge port 12, gas in combustion chamber 1 enters the spiral tube 9 in condensing chamber 2 by production well 7, condensing chamber 2 is provided with water inlet pipe 10 and rising pipe 11, spiral tube 9 space outerpace is filled with cooling medium, cooling medium enters condensing chamber 2 by water inlet pipe 10, rising pipe 11 flows out condensing chamber 2, cooling medium flows in condensing chamber 2, carry out condensation to the gas in spiral tube 9, condensed liquid is collected by discharge port 12 discharging in condensing chamber 2.
Footwall drift germanium device is utilized to the step that waste and old germanium ingot carries out germanium metal recovery method to be: to load in combustion chamber 1 by waste and old germanium ingot by opening for feed 5, utilize well heater 3 by when temperature rises to 400--600 DEG C in combustion chamber 1, Optimal Temperature is 450 DEG C, pass into by the chlorine produced after liquid chlorine vaporization by inlet mouth 4, combustion reactions occurs, and the germanium tetrachloride gas of generation enters the spiral tube 9 in condensing chamber 2 through production well 7.In condensing chamber 2, passed into the salt solution of cooling medium-8 DEG C by water inlet pipe 10, carry out condensation to germanium tetrachloride gas, after condensation, produce liquid is collected by discharge port 12 discharging.
Described well heater 3 is arranged on combustion chamber 1 time, to combustion chamber 1 direct heating, makes temperature in combustion chamber 1 reach 400--600 DEG C, causes chlorine and the burning of waste and old germanium ingot.When combustion reactions occurs, well heater 3 is deactivated.
Add the waste and old germanium ingot of combustion chamber 1 without granularity requirements, pile up more than three pieces in face, 1 same section, combustion chamber simultaneously.Temperature of combustion in combustion chamber 1 controls at 400--600 DEG C, produces germanous chloride when temperature of combustion can be prevented too low; Temperature controls to be regulated by the flow control valve on inlet mouth 4, and pass into Lv Qi Liu Liang Di large-scale combustion temperature higher, chlorine flowrate is excessive causes waste.Production well 7 place on observable dividing plate 8 does not have white smoke to produce, and having in combustion chamber 1 during bright blue flame is optimum temps and chlorine flowrate.
Footwall drift germanium device technique of the present invention is simple, and energy consumption is low, and the germanium rate of recovery is high; Utilize this device to carry out the recovery of germanium metal to waste and old germanium ingot, step is simple, reduces production cost.
Claims (8)
1. a Footwall drift germanium device, it is characterized in that: described device comprises reactor (13) and well heater (3), described reactor (13) is divided into combustion chamber (1) and condensing chamber (2) by dividing plate (8); Described well heater is arranged on combustion chamber (1) bottom, dividing plate (8) is provided with production well (7), combustion chamber (1) is provided with opening for feed (5), and condensing chamber (2) is provided with discharge port (12).
2. a kind of Footwall drift germanium device according to claim 1, it is characterized in that: described combustion chamber (1) is provided with inlet mouth (4), described opening for feed (5) is provided with sealing plug (6).
3. a kind of Footwall drift germanium device according to claim 1, is characterized in that: described condensing chamber (2) is provided with rising pipe (11), water inlet pipe (10).
4. a kind of Footwall drift germanium device according to claim 1-3 any one, it is characterized in that: in described condensing chamber (2), be provided with spiral tube (9), spiral tube (9) one end is connected with production well (7), and the other end is connected with discharge port (12).
5. one kind utilizes the germanium metal recovery method of a kind of Footwall drift germanium device described in claim 4, it is characterized in that: waste and old germanium ingot is loaded by opening for feed (5) in the combustion chamber (1) of reactor (13), seal with sealing plug (6), utilize well heater (3) to after combustion chamber (1) heat temperature raising, pass into chlorine, there is combustion reactions, in the spiral tube (9) of the germanium tetrachloride gas produced in condensing chamber (2), the cooling medium be full of by spiral tube (9) space outerpace is condensed into liquid collecting.
6. germanium metal recovery method according to claim 5, is characterized in that: described cooling medium is the salt solution of-8 DEG C.
7. germanium metal recovery method according to claim 5, it is characterized in that: described well heater (3) is heated to combustion chamber (1) interior temperature to combustion chamber (1) and reaches 400--600 DEG C, cause chlorine and the burning of waste and old germanium ingot.
8. germanium metal recovery method according to claim 5, is characterized in that: described well heater (3), when passing into chlorine generation combustion reactions, is deactivated.
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| CN201510299886.9A CN104862500A (en) | 2015-06-03 | 2015-06-03 | Metal germanium recovery device and metal germanium recovery method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756028A (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 germanium tetrachloride production apparatus for recovering metal |
| RU2658546C2 (en) * | 2016-09-09 | 2018-06-21 | Елена Алексеевна Строганова | Method for processing a zinc and copper-containing polymetallic mineral material |
| CN110079686A (en) * | 2018-11-20 | 2019-08-02 | 云南驰宏国际锗业有限公司 | A kind of germanium scrap metal processing method |
| CN115477322A (en) * | 2022-09-29 | 2022-12-16 | 云南驰宏国际锗业有限公司 | Ultra-high purity GeCl 4 Preparation method |
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| CN204714876U (en) * | 2015-06-03 | 2015-10-21 | 云南天浩稀贵金属股份有限公司 | A kind of device of chlorine combustion method Footwall drift germanium |
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2015
- 2015-06-03 CN CN201510299886.9A patent/CN104862500A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756028A (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 germanium tetrachloride production apparatus for recovering metal |
| RU2658546C2 (en) * | 2016-09-09 | 2018-06-21 | Елена Алексеевна Строганова | Method for processing a zinc and copper-containing polymetallic mineral material |
| CN110079686A (en) * | 2018-11-20 | 2019-08-02 | 云南驰宏国际锗业有限公司 | A kind of germanium scrap metal processing method |
| CN115477322A (en) * | 2022-09-29 | 2022-12-16 | 云南驰宏国际锗业有限公司 | Ultra-high purity GeCl 4 Preparation method |
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Application publication date: 20150826 |