CN106367619A - Recovery method for germanium in grinding wastewater of germanium wafers - Google Patents

Recovery method for germanium in grinding wastewater of germanium wafers Download PDF

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Publication number
CN106367619A
CN106367619A CN201610839787.XA CN201610839787A CN106367619A CN 106367619 A CN106367619 A CN 106367619A CN 201610839787 A CN201610839787 A CN 201610839787A CN 106367619 A CN106367619 A CN 106367619A
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germanium
reverse osmosis
water
recovery method
fresh water
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李琴香
朱刘
王文杰
王晓玲
孙秋景
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Vital Materials Co Ltd
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Vital Materials 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
    • C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical 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
    • 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
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/346—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from semiconductor processing, e.g. waste water from polishing of wafers
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
    • 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
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention provides a recovery method for germanium in grinding wastewater of germanium wafers. The method comprises the following steps that A, under the condition that the pH value ranges from 5 to 10, molysite and germanium elements in the wastewater are subjected to precipitation reaction, filtration is conducted, and germanium concentrate and filtrate are obtained; B, the filtrate is sequentially subjected to precise filtration and primary reverse osmosis, and first fresh water and first concentrated water are obtained; C, the first concentrated water is subjected to treatment of step A, the first fresh water is subjected to secondary reverse osmosis, and second fresh water and second concentrated water are obtained; and D, the second concentrated water is subjected to treatment of step B, and the second fresh water is recovered. The provided method is simple in process, short in time and high in automation degree, chemical reagents are easy to obtain, quite few precipitators are used, and the high precipitation rate and recovery rate can be achieved; and the content of recovered germanium in germanium concentrate is higher than or equal to 3%, and the fresh water subjected to film equipment treatment can be reused.

Description

The recovery method of germanium in a kind of germanium wafer abrasive waste water
Technical field
The present invention relates to technical field of wet metallurgy, the recovery method of germanium in more particularly, to a kind of germanium wafer abrasive waste water.
Background technology
Germanium wafer is a kind of new clean energy resource material, and the operation such as cleaved-to grind-corrosion-polishing can be processed into germanium list Brilliant polished silicon wafer, wherein process of lapping can produce substantial amounts of waste water, and the germanium comprising in waste water is one of important dissipated metal.From complete From the point of view of the purposes of ball, the application of germanium is transferred to infrared, optical fiber, chemical industry from the semiconductor device of traditional manufacture electronics industry and is urged Agent and solar cell material.Germanium leads to it to extract difficulty greatly due to its high dispersion, and its value is sufficiently expensive, because And each enterprises and institutions all take much count of extraction and the recovery of germanium always.
And according to different content in different material for the germanium and different physical forms, extract method also each not phase of germanium With.A kind of method of microwave pretreatment Ti recovery from germanium oxide dust is disclosed, it is suitable in such as patent No. cn102345021 In germanium-containing smoke dust, the mass percent of germanium is 0.04%～1% germanium oxide dust.
Research worker is also had to adopt chelating agent to extract, the method for alkali back extraction reaches the enrichment of germanium, but this method is only applicable to germanium Concentration is higher than the solution of 30mg/l.
In above-mentioned germanium wafer abrasive waste water, the particle diameter of germanium is very little, is distributed between 0.01～0.5 micron, grinds in high speed With air contact during mill, the germanium grinding can be oxidized, and is dissolved in waste water, and the concentration of germanium is very low, only 10ppm～100ppm.Said method is all inapplicable.The technique of existing Ti recovery has that technological process is long, and time-consuming, cost Height, the relatively low problem of the response rate, up to the present, not be applied to germanium wafer abrasive waste water germanium recovery process.
Therefore, exigence develop a kind of process is simple, time-consuming short, high degree of automation, the easy to operate, response rate high and Reclaim slag in germanium content >=3% be applied to germanium abrasive waste water germanium recovery method.
Content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of recovery side of germanium in germanium wafer abrasive waste water Method, has the higher response rate, and time-consuming short.
The invention provides in a kind of germanium wafer abrasive waste water germanium recovery method, comprise the following steps:
A) under conditions of ph value is for 5～10, coprecipitation reaction is carried out with the Ge element in waste water using iron salt, filters, Obtain germanium concentrate and filtrate；
B) filtrate sequentially passes through secondary filter and first-stage reverse osmosis, obtains the first fresh water and the first concentrated water；
C) the first concentrated water return to step a)；First fresh water, through two-pass reverse osmosis, obtains the second fresh water and the second concentrated water；
D) the second concentrated water return to step b), the second fresh water reclaims.
Preferably, described iron salt is fecl3Or fe2(so4)3.
Preferably, in described iron salt, the quality of ferrum element and the mass ratio of Ge element in waste water are (5～15): 1.
Preferably, the time of described reaction is 0.5～2h.
Preferably, in described germanium wafer abrasive waste water, the content of germanium is 10ppm～100ppm.
Preferably, in described germanium concentrate, Ge content is more than or equal to 3%.
Preferably, described first-stage reverse osmosis adopt Tao Shi bitter film bw30-4040.
Preferably, described two-pass reverse osmosis adopt Tao Shi ultra-low-pressure reverse osmosis film lp-4040.
Compared with prior art, the invention provides in a kind of germanium wafer abrasive waste water germanium recovery method, including following Step: a) under conditions of ph value is for 5～10, coprecipitation reaction is carried out with the Ge element in waste water using iron salt, filter, obtain Germanium concentrate and filtrate；B) filtrate sequentially passes through secondary filter and first-stage reverse osmosis, obtains the first fresh water and the first concentrated water；C) first Concentrated water return to step a)；First fresh water, through two-pass reverse osmosis, obtains the second fresh water and the second concentrated water；D) the second concentrated water returns step Suddenly b), the second fresh water reclaims.Method process is simple that the present invention provides, take short, high degree of automation, chemical reagent used It is easy to get, using considerably less precipitant, you can obtain higher rate of deposition and the response rate, and reclaimed germanium in the germanium concentrate obtaining Content >=3%.Fresh water after film device is processed can reuse.
Brief description
The process chart of the recovery method that Fig. 1 provides for the present invention.
Specific embodiment
The invention provides in a kind of germanium wafer abrasive waste water germanium recovery method, comprise the following steps:
A) under conditions of ph value is for 5～10, coprecipitation reaction is carried out with the Ge element in waste water using iron salt, filters, Obtain germanium concentrate and filtrate；
B) filtrate sequentially passes through secondary filter and first-stage reverse osmosis, obtains the first fresh water and the first concentrated water；
C) the first concentrated water return to step a)；First fresh water, through two-pass reverse osmosis, obtains the second fresh water and the second concentrated water；
D) the second concentrated water return to step b), the second fresh water reclaims.
Its process chart is shown in Fig. 1.
Said method process is simple, time-consuming short, high degree of automation, chemical reagent used is easy to get, using considerably less Precipitant, you can obtain higher rate of deposition and the response rate, and reclaimed content >=3% of germanium in the germanium concentrate obtaining.Through Fresh water after film device is processed can reuse.
In germanium wafer abrasive waste water of the present invention, Ge content is preferably 10ppm～100ppm, and the particle diameter of germanium is preferably 0.01 μm～0.5 μm.
The iron salt being adopted is preferably fecl3Or fe2(so4)3, in some embodiments of the invention, using fecl3 Aqueous solution, its concentration be preferably 30%～50%, in some embodiments of the invention, its concentration be 36%.
In described iron salt, the quality of ferrum element and the mass ratio of Ge element in waste water are preferably (5～15): 1.
Present invention preferably employs alkali compoundss regulation system ph value is to 5～10, described alkali compoundss are preferably naoh Or koh, in certain embodiments of the present invention, solution ph is adjusted using 30%naoh aqueous solution.
The time of described coprecipitation reaction is preferably 0.5～2h.
After reaction terminates, preferably standing a period of time, then filter.Present invention preferably employs the method for filter pressing.
The solid filtering is germanium concentrate, and wherein, Ge content is more than or equal to 3%.
Currently preferred, drying and processing is carried out to described germanium concentrate.
In the filtrate filtered, Ge content is 1～10ppm, carries out secondary filter to it, preferably by filtrate through secondary filter Device, particle or macromole that retention size is more than 0.5 μm.
Then carry out first-stage reverse osmosis, preferably solution is pressed into first-stage reverse osmosis film device, described first-stage reverse osmosis film sets Standby preferably reverse osmosis membrane system+edi pure water system.
Most preferably, described first-stage reverse osmosis adopt Tao Shi bitter film bw30-4040.
Obtain the first fresh water and the first concentrated water.
Wherein, in the first concentrated water, Ge content is higher than 10ppm, and its return to step a) carries out second coprecipitation reaction.
In first fresh water, Ge content is less than 10ppm, and it proceeds two-pass reverse osmosis, preferably solution is pressed into two grades instead Infiltration film device, described two-pass reverse osmosis film device is preferably reverse osmosis membrane system+edi pure water system.
Most preferably, described two-pass reverse osmosis adopt Tao Shi ultra-low-pressure reverse osmosis film lp-4040.
Obtain the second fresh water and the second concentrated water.
Wherein, in the second concentrated water, Ge content is higher than 1ppm, and its return to step b) carries out second first-stage reverse osmosis.
In second fresh water, Ge content is 0.1～0.3ppm, and it can directly reclaim secondary utilization.
The present invention passes through Tao Shi bitter film bw30-4040, and Tao Shi ultra-low-pressure reverse osmosis film lp-4040 applies mechanically, twice Reverse osmosiss, it becomes possible to make Ge content reach 0.1～0.3ppm, meet waste water reclamation standard, and technological process is short, have preferably Economic benefit.
The recovery method that the present invention provides, had both carried out germanium to the germanic abrasive waste water producing in germanium wafer process of lapping and had returned Receive, achieve useless water purification and recycling again.
In order to further illustrate the present invention, with reference to germanium in the germanium wafer abrasive waste water that embodiment provides to the present invention Recovery method is described in detail.
In following embodiments, first-stage reverse osmosis film is Tao Shi bitter film bw30-4040, and two-pass reverse osmosis film surpasses for Tao Shi Low-pressure reverse osmosis membrane lp-4040.
Embodiment 1
Take the germanic abrasive waste water 15l that Ge content is 14ppm in coprecipitation reaction kettle, add 36% fecl3Solution After 11g, stir, add 30%naoh solution to adjust ph to 6.87, react 30 minutes, standing filtered after 10 minutes.Filtering residue Dry, obtain the germanium concentrate 2.4g that Ge content is 7.5%, the rate of deposition 85.7% of germanium.
In filtrate, the content of germanium is 2ppm, and filtrate initially enters accurate filter, intercepts the particle that size is more than 0.5 micron Or colloid, subsequently into first-stage reverse osmosis film, respectively obtaining the concentrated water that 2l Ge content is 10ppm and 13l Ge content is 0.7ppm Fresh water, 2l concentrated water enter together with stock solution carry out in coprecipitation reaction kettle co-precipitation operation.13l fresh water enters two-pass reverse osmosis Film, obtains the germanic concentrated water of 2l 4ppm and the fresh water of 11l 0.1ppm.Concentrated water is back in first-stage reverse osmosis film, and fresh water can return With.
Embodiment 2
Take the germanic abrasive waste water 15l that Ge content is 35.6ppm in coprecipitation reaction kettle, add 36% fecl3Molten After liquid 20g, stir, add 30%naoh solution to adjust ph to 6.4, react 30 minutes, standing filtered after 10 minutes.Filtering residue Dry, obtain the germanium concentrate 4.0392g that Ge content is 9.0%, the rate of deposition 86.5% of germanium.
In filtrate, the content of germanium is 4.8ppm, and filtrate initially enters accurate filter, intercepts the grain that size is more than 0.5 micron Son or colloid, subsequently into first-stage reverse osmosis film, respectively obtain the concentrated water that 2l Ge content is 25ppm and 13l Ge content are The fresh water of 1.7ppm, 2l concentrated water is entered together with stock solution and carries out co-precipitation operation in coprecipitation reaction kettle.13l fresh water enters two grades Reverse osmosis membrane, obtains the germanic concentrated water of 2l 10ppm and the fresh water of 11l 0.2ppm.Concentrated water is back in first-stage reverse osmosis film, light Water can reuse.
Embodiment 3
Take the germanic abrasive waste water 15l that Ge content is 50ppm in coprecipitation reaction kettle, add 36% fecl3Solution After 30g, stir, add 30%naoh solution to adjust ph to 6.99, react 30 minutes, standing filtered after 10 minutes.Filtering residue Dry, obtain the germanium concentrate 6.4545g that Ge content is 11%, the rate of deposition 94.6% of germanium.
In filtrate, the content of germanium is 2.68ppm, and filtrate initially enters accurate filter, intercepts size and is more than 0.5 micron Particle or colloid, subsequently into first-stage reverse osmosis film, respectively obtain the concentrated water that 2l Ge content is 12ppm and 13l Ge content are The fresh water of 1.25ppm, 2l concentrated water is entered together with stock solution and carries out co-precipitation operation in coprecipitation reaction kettle.13l fresh water enters two Level reverse osmosis membrane, obtains the germanic concentrated water of 2l 7ppm and the fresh water of 11l 0.2ppm.Concentrated water is back in first-stage reverse osmosis film, Fresh water can reuse.
The recovery method of the germanium being provided from above-described embodiment, the present invention, the response rate is higher, and time-consuming shorter, 1～ 2h can complete.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that it is right For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out Some improvement and modification, these improve and modify and also fall in the protection domain of the claims in the present invention.

Claims (8)

1. in a kind of germanium wafer abrasive waste water the recovery method of germanium it is characterised in that comprising the following steps:
A) under conditions of ph value is for 5～10, coprecipitation reaction is carried out with the Ge element in waste water using iron salt, filter, obtain Germanium concentrate and filtrate；
B) filtrate sequentially passes through secondary filter and first-stage reverse osmosis, obtains the first fresh water and the first concentrated water；
C) the first concentrated water return to step a)；First fresh water, through two-pass reverse osmosis, obtains the second fresh water and the second concentrated water；
D) the second concentrated water return to step b), the second fresh water reclaims.
2. recovery method according to claim 1 is it is characterised in that described iron salt is fecl3Or fe2(so4)3.
3. recovery method according to claim 1 is it is characterised in that germanium in the quality of ferrum element and waste water in described iron salt The mass ratio of element is (5～15): 1.
4. recovery method according to claim 1 is it is characterised in that the time of described reaction is 0.5～2h.
5. recovery method according to claim 1 it is characterised in that in described germanium wafer abrasive waste water the content of germanium be 10ppm～100ppm.
6. recovery method according to claim 1 is it is characterised in that in described germanium concentrate, Ge content is more than or equal to 3%.
7. recovery method according to claim 1 is it is characterised in that described first-stage reverse osmosis adopt Tao Shi bitter film bw30-4040.
8. recovery method according to claim 1 is it is characterised in that described two-pass reverse osmosis adopt Tao Shi ultralow pressure reverse osmosis Permeable membrane lp-4040.
CN201610839787.XA 2016-09-21 2016-09-21 Recovery method for germanium in grinding wastewater of germanium wafers Pending CN106367619A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110922006A (en) * 2019-12-18 2020-03-27 云南驰宏国际锗业有限公司 Germanium mud pretreatment method
CN114314925A (en) * 2021-12-30 2022-04-12 广东先导微电子科技有限公司 Treatment method of germanium thinning process processing wastewater

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101205572A (en) * 2007-12-03 2008-06-25 云南驰宏锌锗股份有限公司 Technique for extracting germanium from germanium-containing material by pressure leaching
CN102259960A (en) * 2011-04-25 2011-11-30 北京通美晶体技术有限公司 Method for separating germanium particles from wastewater containing fine granular germanium
WO2016055372A1 (en) * 2014-10-06 2016-04-14 Emmanuel Trouve Device and method for recovering a precipitated solid inorganic final product consisting of phosphorus, nitrogen and an element x

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101205572A (en) * 2007-12-03 2008-06-25 云南驰宏锌锗股份有限公司 Technique for extracting germanium from germanium-containing material by pressure leaching
CN102259960A (en) * 2011-04-25 2011-11-30 北京通美晶体技术有限公司 Method for separating germanium particles from wastewater containing fine granular germanium
WO2016055372A1 (en) * 2014-10-06 2016-04-14 Emmanuel Trouve Device and method for recovering a precipitated solid inorganic final product consisting of phosphorus, nitrogen and an element x

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110922006A (en) * 2019-12-18 2020-03-27 云南驰宏国际锗业有限公司 Germanium mud pretreatment method
CN114314925A (en) * 2021-12-30 2022-04-12 广东先导微电子科技有限公司 Treatment method of germanium thinning process processing wastewater

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