CN106906364A - The process of Ti recovery from germanic fluorine containing corrosion liquid - Google Patents

The process of Ti recovery from germanic fluorine containing corrosion liquid Download PDF

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Publication number
CN106906364A
CN106906364A CN201710131082.7A CN201710131082A CN106906364A CN 106906364 A CN106906364 A CN 106906364A CN 201710131082 A CN201710131082 A CN 201710131082A CN 106906364 A CN106906364 A CN 106906364A
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fluorine
germanium
germanic
liquid
recovery
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CN201710131082.7A
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CN106906364B (en
Inventor
普世坤
朱知国
窦辉
李璇
薛丹
吴王昌
李正美
滕文
谢高
杨再磊
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Yunnan Dongchang metal processing Co., Ltd
YUNNAN LINCANG XINYUAN GERMANIUM INDUSTRY CO LTD
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YUNNAN DONGCHANG METAL PROCESSING CO Ltd
YUNNAN LINCANG XINYUAN GERMANIUM CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B41/00—Obtaining germanium
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The process of Ti recovery from germanic fluorine containing corrosion liquid, is related to technical field of wet metallurgy, specially a kind of to sink germanium fluorine removal, the method for silica fluorine removal come the process of Ti recovery using boric acid from germanic fluorine containing corrosion liquid.The process of the Ti recovery from germanic fluorine containing corrosion liquid of the invention, it is characterised in that simultaneously using boric acid and silica is added, heating volatilization removes fluorine and precipitate enriched germanium and carrys out Ti recovery metal the process.Fluoride removing rate of the present invention is up to more than 78%, it is fluorine-containing in the final germanic slag being transferred in chlorinated distillation step and raffinate to be less than 0.05%, precipitation obtains germanium cinder grade up to more than 25%, the germanium rate of recovery can reach more than 95% before being wherein transferred to chlorinated distillation, and the loss late of germanium metal is less than 1.2% during whole fluorine removal；Part supernatant waste liquid wherein after fluorine removal carries out the secondary heavy germanium treatment of circulation and stress.In the chlorinated distillation of germanic slag and raffinate is carried out, the steam rate of germanium can reach more than 98%, can meet manufacturing technique requirent.

Description

The process of Ti recovery from germanic fluorine containing corrosion liquid
Technical field
The present invention relates to technical field of wet metallurgy, specially one kind is removed from germanic fluorine containing corrosion liquid using the heavy germanium of boric acid Fluorine, the method for silica fluorine removal carry out the process of Ti recovery from germanic fluorine containing corrosion liquid of Ti recovery.
Background technology
Germanium belongs to rare scattering elements, and critical role is occupied in national defense and military and modern science and technology, and optical fiber leads to Credit germanium, infrared optics germanium, used in electronic industry germanium, Medicines and Health Product germanium, superconductor germanium, photoelectric source germanium etc. are all Important use of the germanium in every field.And germanium resource is limited, the germanium resource amount that can be exploited as germanium ore deposit is even more little, institute With by germanium smelt and process of manufacture in the germanium waste material that produces, waste liquid carry out germanium recovery, so as to realize germanium waste material, germanium waste liquid Germanium resourceization is significant.
Often along with a large amount of generations containing germanium waste material, waste liquid, germanium Product processing is got over to rear end for the smelting and production and processing of germanium The germanic waste recovery for producing is more complicated various.Wherein, chemical corruption is carried out to metal surfaces such as metal germanium ingots in processing The mixed acid of hydrofluoric acid and nitric acid has been used during erosion polishing carries out oxidation processes, just generates fluorine-containing, germanic corrosive liquid high, because Corrosive liquid is fluorine-containing too high, the corrosion distillation equipment such as rectifying, it is impossible to directly using chlorization distillation method treatment, therefore causes this fluorine-containing to contain Germanium corrosive liquid difficult treatment, germanium cost recovery is high.
The content of the invention
Exactly existing height to be solved by this invention is fluorine-containing, germanic corrosive liquid can corrode distillation rectifying device, causes treatment Difficulty, germanium cost recovery problem high, there is provided one kind is removed from germanic fluorine containing corrosion liquid using the heavy germanium fluorine removal of boric acid, silica The method of fluorine carrys out the process of Ti recovery.
The process of the Ti recovery from germanic fluorine containing corrosion liquid of the invention, it is characterised in that the process is adopted simultaneously With boric acid and silica is added, heating volatilization removes fluorine and precipitates enriched germanium and carrys out Ti recovery metal, and concrete technology step is such as Under：
The first step：Appropriate germanic fluorine containing corrosion waste liquid is taken, is put into polytetrafluoroethylcontainer container, measured the fluorine that the corrosive liquid contains and contain Amount and Ge content, are calculated the fluorine quality in waste liquid for A and germanium quality are B, and it is D's for the boric acid and quality of C to add quality Silica, is stirred after mixing, and polytetrafluoroethylcontainer container is connected with waste gas reception device, is equipped with waste gas reception device The watery hydrochloric acid of 1-2mol/L is used as waste gas reception liquid；
Second step, heats polytetrafluoroethylcontainer container, continues to stir the carrying out to promote to be chemically reacted in solution, heated solution temperature To 80-90 DEG C, the duration of heat is 15-30 min；
3rd step, after heating terminates, takes the supernatant liquor part in polytetrafluoroethylcontainer container, remaining residual night, residue and waste gas Reception liquid is standby；
4th step, clear liquid adds appropriate germanic fluorine containing corrosion waste liquid in the 3rd step, repeats the first step, second step process, will obtain Raffinate, the raffinate that is obtained with the 3rd step of residue, residue mixed；
5th step, the residue obtained after the 4th step is mixed, raffinate are transferred in distillation reaction bottle, add the dense salt of 10mol/L Acid, by conventional chlorinating distillating method Ti recovery metal.
Described boric acid quality C is 1.5 to 3 times of the fluorine quality A in waste liquid, and silica quality D is the fluorine in waste liquid 0.2 to 0.4 times of quality A.
The reaction equation of above-mentioned process is：
3F-+H3BO3+3H+ =BF3↑+3H2O ………………（1）
4F-+SiO2+4H+ = SiF4↑+2H2O ……………………（2）.
Described waste gas reception liquid is the dilute hydrochloric acid solution of 1-2mol/L.
The process of the Ti recovery from germanic fluorine containing corrosion liquid of the invention, step is simple, and convenient and practical, fluoride removing rate can Up to more than 78%, fluorine-containing in the germanic slag and raffinate that are finally transferred in chlorinated distillation step to be less than 0.05%, precipitation obtains germanium slag product Position is up to more than 25%, wherein being transferred to the germanium rate of recovery before chlorinated distillation can reach more than 95%, and germanium metal during whole fluorine removal Loss late be less than 1.2%；Part supernatant waste liquid wherein after fluorine removal carries out the secondary heavy germanium treatment of circulation and stress.Carry out it is germanic In the chlorinated distillation of slag and raffinate, the steam rate of germanium can reach more than 98%, can meet manufacturing technique requirent.Preferably solve The recovery problem of germanium in germanic fluorine containing corrosion liquid.
Specific embodiment
Embodiment 1：A kind of process of the Ti recovery from germanic fluorine containing corrosion liquid, using addition boric acid and titanium dioxide Silicon, heating volatilization removes fluorine and precipitates enriched germanium and carrys out Ti recovery metal, and concrete technology step is as follows：
The first step：The germanic fluorine containing corrosion liquid of 500mL is taken, is put into polytetrafluoroethylcontainer container, measure the Oil repellent that the corrosion contains 45.80g/L and 26.45 g/L are respectively with Ge content, fluorine quality is calculated for 22.9g, germanium quality is 13.225g, is added Boric acid 45.80g and silica 4.58g, is stirred after mixing, and polytetrafluoroethylcontainer container is connected with waste gas reception device, Equipped with the waste gas reception liquid of the dilute hydrochloric acid solution that 200mL concentration is 1mol/L in waste gas reception device；
Second step, heats polytetrafluoroethylcontainer container, continues to stir to promote the generation of solution reaction, heated solution temperature to 80- 90 DEG C, the duration of heat is 15min；
3rd step, after heating terminates, takes the supernatant liquor part in polytetrafluoroethylcontainer container, remaining residual night, residue and waste gas Reception liquid is standby；Waste gas containing fluoride reception liquid is cooled to room temperature, is settled in 250 mL volumetric flasks, contained in detection waste gas reception liquid Germanium, fluorinated volume；Residue precipitation raffinate and precipitation slag are separated, germanic, fluorinated volume therein is detected respectively.Testing result：Waste gas Germanic 2.80 g/L in reception liquid, account for the 0.53% of total germanium, fluorine-containing 73.26 g/L, account for 79.98 % of total fluorine；Contain in precipitation raffinate The g/L of germanium 12.5, account for the 3% of total germanium, fluorine-containing 28.75 g/L, account for the 0.040% of total fluorine；Fluorine-containing 1.98%, germanium grade in precipitating residue Up to 29.43%；
4th step, clear liquid adds appropriate germanic fluorine containing corrosion liquid in the 3rd step, the first step, second step process is repeated, by what is obtained Raffinate that raffinate, residue are obtained with the 3rd step, residue are mixed, and calculate that fluoride removing rate is 80% and heavy germanium rate is 95%, germanium accordingly The rate of recovery is 96%；
5th step, the residue obtained after the 4th step is mixed, raffinate are transferred in cucurbit, add the concentrated hydrochloric acid of 10mol/L, are led to Cross traditional chlorinated distillating method Ti recovery metal, steam rate is up to 98.5%.
Embodiment 2：A kind of process of the Ti recovery from germanic fluorine containing corrosion liquid, using addition boric acid and titanium dioxide Silicon, heating volatilization removes fluorine and precipitates enriched germanium and carrys out Ti recovery metal, and concrete technology step is as follows：
The first step：The germanic fluorine containing corrosion liquid of 500mL is taken, is put into polytetrafluoroethylcontainer container, measure the Oil repellent that the corrosion contains 51.83 g/L and 28.99 g/L are respectively with Ge content, fluorine quality is calculated for 25.915g, germanium quality is 14.495g, plus Enter boric acid 38.873g and silica 7.77g, stirred after mixing, polytetrafluoroethylcontainer container and waste gas reception device are connected Connect, equipped with the waste gas reception liquid that 200mL concentration is 2 mol/L dilute hydrochloric acid solutions in waste gas receiving device；
Second step, heats polytetrafluoroethylcontainer container, continues to stir to promote the generation of solution reaction, heated solution temperature to 80- 90 DEG C, the duration of heat is 30min；
3rd step, after heating terminates, takes the supernatant liquor part in polytetrafluoroethylcontainer container, remaining raffinate, residue and waste gas Reception liquid is standby；Waste gas containing fluoride reception liquid is cooled to room temperature, is settled in 250 mL volumetric flasks, contained in detection waste gas reception liquid Germanium, fluorinated volume；Residue precipitation raffinate and precipitation slag are separated, germanic, fluorinated volume therein is detected respectively.Testing result：Waste gas Germanic 2.61 g/L in reception liquid, account for the 0.45% of total germanium, fluorine-containing 82.94 g/L, account for the 80.01% of total fluorine；Contain in precipitation raffinate The g/L of germanium 14.29, account for the 3.45% of total germanium, fluorine-containing 41.43 g/L, account for the 0.056% of total fluorine；Fluorine-containing 1.77% in precipitating residue, contain Germanium grade is up to 31.3%；
4th step, clear liquid adds appropriate germanic fluorine containing corrosion liquid in the 3rd step, the first step, second step process is repeated, by what is obtained Raffinate that raffinate, residue are obtained with the 3rd step, residue are mixed, and calculate that fluoride removing rate is 80% and heavy germanium rate is 95%, germanium accordingly The rate of recovery is 97%；
5th step, the residue obtained after the 4th step is mixed, raffinate are transferred in cucurbit, concentrated hydrochloric acid are added, by traditional chlorine Change distillating method Ti recovery metal, steam rate is up to 98.8%.

Claims (3)

1. a kind of process of the Ti recovery from germanic fluorine containing corrosion liquid, it is characterised in that the process is using adding boric acid And silica, heating volatilization, removing fluorine and precipitate enriched germanium and carry out Ti recovery metal, concrete technology step is as follows：
The first step：Appropriate germanic fluorine containing corrosion waste liquid is taken, is put into polytetrafluoroethylcontainer container, measure the Oil repellent that the corrosion contains And Ge content, the fluorine quality in waste liquid is calculated for A and germanium quality are B, it is the two of D for the boric acid and quality of C to add quality Silica, is stirred after mixing, and polytetrafluoroethylcontainer container is connected with waste gas reception device, equipped with useless in waste gas receiving device Gas reception liquid；
Second step, heats polytetrafluoroethylcontainer container, continues to stir to promote the generation of solution reaction, heated solution temperature to 80- 90 DEG C, the duration of heat is 15-30 min；
3rd step, after heating terminates, takes the supernatant liquor part in polytetrafluoroethylcontainer container, remaining raffinate, residue and waste gas Reception liquid is standby；
4th step, clear liquid adds appropriate germanic fluorine containing corrosion liquid in the 3rd step, the first step, second step process is repeated, by what is obtained Raffinate that residual night, residue are obtained with the 3rd step, residue are mixed；
5th step, the residue obtained after the 4th step is mixed, raffinate are transferred in cucurbit, add the concentrated hydrochloric acid of 10mol/L, are led to Cross traditional chlorinated distillating method Ti recovery metal.
2. the boric acid quality C described in is 1.5 to 3 times of the fluorine quality A in waste liquid, and silica quality D is the fluorine matter in waste liquid 0.2 to 0.4 times of amount A.
3. the process of the Ti recovery from germanic fluorine containing corrosion liquid as claimed in claim 1, it is characterised in that described is useless Gas reception liquid is the dilute hydrochloric acid solution of 1-2mol/L.
CN201710131082.7A 2017-03-07 2017-03-07 The process of Ti recovery from germanic fluorine containing corrosion liquid Active CN106906364B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097603A (en) * 2018-09-12 2018-12-28 云南临沧鑫圆锗业股份有限公司 The process of Ti recovery from germanium wafer intensive processing spent acid
CN110453097A (en) * 2019-09-17 2019-11-15 广东先导稀材股份有限公司 A method of germanium is extracted in distillation from fluorine-containing germanium concentrate

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CN101418373A (en) * 2008-09-16 2009-04-29 云南临沧鑫圆锗业股份有限公司 Method for extracting germanium from chlorinated distillation slag
WO2009106660A1 (en) * 2008-02-28 2009-09-03 Universidad De Sevilla Method for the recovery of germanium in solution by means of complexing and use of ion-exchange resins
CN103757422A (en) * 2014-02-19 2014-04-30 云南东昌金属加工有限公司 Method for recovering germanium from germanium-containing multi-metal material
CN104818397A (en) * 2015-05-19 2015-08-05 河北工程大学 Method for extracting germanium from coal
CN105821224A (en) * 2016-06-06 2016-08-03 云南临沧鑫圆锗业股份有限公司 Method for extracting germanium in low-grade germanium concentrates through fluoride roasting process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009106660A1 (en) * 2008-02-28 2009-09-03 Universidad De Sevilla Method for the recovery of germanium in solution by means of complexing and use of ion-exchange resins
CN101418373A (en) * 2008-09-16 2009-04-29 云南临沧鑫圆锗业股份有限公司 Method for extracting germanium from chlorinated distillation slag
CN103757422A (en) * 2014-02-19 2014-04-30 云南东昌金属加工有限公司 Method for recovering germanium from germanium-containing multi-metal material
CN104818397A (en) * 2015-05-19 2015-08-05 河北工程大学 Method for extracting germanium from coal
CN105821224A (en) * 2016-06-06 2016-08-03 云南临沧鑫圆锗业股份有限公司 Method for extracting germanium in low-grade germanium concentrates through fluoride roasting process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097603A (en) * 2018-09-12 2018-12-28 云南临沧鑫圆锗业股份有限公司 The process of Ti recovery from germanium wafer intensive processing spent acid
CN109097603B (en) * 2018-09-12 2020-11-06 云南临沧鑫圆锗业股份有限公司 Process method for recovering germanium from germanium wafer deep processing waste acid
CN110453097A (en) * 2019-09-17 2019-11-15 广东先导稀材股份有限公司 A method of germanium is extracted in distillation from fluorine-containing germanium concentrate
CN110453097B (en) * 2019-09-17 2021-12-17 广东先导稀材股份有限公司 Method for distilling and extracting germanium from fluorine-containing germanium concentrate

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