CN106702429A - Method for purifying and recovering caustic alkali for producing metal gallium through alkaline method - Google Patents
Method for purifying and recovering caustic alkali for producing metal gallium through alkaline method Download PDFInfo
- Publication number
- CN106702429A CN106702429A CN201611197219.0A CN201611197219A CN106702429A CN 106702429 A CN106702429 A CN 106702429A CN 201611197219 A CN201611197219 A CN 201611197219A CN 106702429 A CN106702429 A CN 106702429A
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- Prior art keywords
- precipitation process
- section
- tail washings
- precipitation
- caustic alkali
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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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
- 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 Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a method for purifying and recovering caustic alkali for producing metal gallium through an alkaline method. A precipitator containing barium ion salt or alkali is added into a new electrolyte solution, and the molar mass ratio of sulfate radicals to barium ions in the new electrolyte tail solution is 1: (0.8 to 1.4). The method for purifying and recovering the caustic alkali for producing the metal gallium through the alkaline method has the beneficial effects that not only can the sulfate radicals be eradicated, but also metal vanadium can be removed for purifying the electrolyte tail solution, so that the caustic alkali can be recovered as much as possible, and the aim of reducing the production cost is achieved.
Description
Technical field
It is severe the present invention relates to alkaline process production gallium tail washings purification techniques field, more particularly to a kind of alkaline process production gallium
Property alkaline purification reclaim method.
Background technology
, it is necessary to the use of a large amount of caustic alkali be liquid caustic soda, year consumption can reach during prior art alkaline process production gallium
To 12000 tons, in order to cost-effective, these caustic alkali are by being electrolysed the form major part recycling use of tail washings.In alkaline process
In production technology, system can constantly produce sulfate radical and newly-increased certain amount vanadium metal, as electrolysis tail washings is constantly recycled,
Sulfate radical and vanadium metal are constantly accumulated in electrolysis tail washings, so as to produce significant impact to system.Its influence includes：Crystallization is refined,
Cannot filter；Electrolytic efficiency significantly declines, and power consumption increases；Gallium rate of recovery reduction, yield declines.Therefore in the prior art when
Sulfate radical content is 30-60g/L in electrolysis tail washings, it is necessary to tail washings is drained one when the content of vanadium metal is 15-60mg/L
Point, the concentration of sulfate radical and vanadium metal in reduction system supplements part caustic alkali to maintain normally to produce needs.To mend every year
1800-2000 tons of caustic alkali in system is charged to, value 4,500,000 or so, is the production cost main composition of gallium.
Therefore prior art has much room for improvement and develops.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind and vanadium metal can also can be removed with net sulfate radical removing
Change electrolysis tail washings, it is as far as possible to reclaim caustic alkali more, so that the alkaline process production gallium causticity alkaline purification for reducing production cost is returned
The method of receipts.
Technical solution of the invention is：The method that alkaline process produces gallium caustic alkali Recovery Purifying, will contain barium ions
The precipitating reagent of salt or alkali is added in new electrolyte, the molal weight of sulfate radical and the barium ions in the new electrolysis tail washings
Than being 1:(0.8-1.4).
The precipitating reagent is added to the new electrolysis tail washings using three sections of adverse current place of settling logos；
Wherein first paragraph precipitation process is carried out using two sections of precipitating reagents that second segment precipitation process is obtained to new electrolysis tail washings
Precipitation, to obtain one section of tail washings；
Second segment precipitation process is precipitated using one section of precipitating reagent to one section of tail washings；To obtain two sections of tail washings and two sections
Precipitating reagent；
3rd section of precipitation process is precipitated using new precipitating reagent to two sections of tail washings；To obtain qualified tail washings and second segment
One section of precipitating reagent needed for precipitation process.
It in temperature is 30-50 DEG C that first paragraph precipitation process, second segment precipitation process and the 3rd section of precipitation process are
Under the conditions of carry out.
It is small that the reaction time of first paragraph precipitation process, second segment precipitation process and the 3rd section of precipitation process is 0.5-4
When.
The precipitation mixing time of first paragraph precipitation process, second segment precipitation process and the 3rd section of precipitation process is 1-3
Hour.
Beneficial effects of the present invention：
Under the solution system of highly basic, using a kind of barium salt or alkali for dissolving in strong base solution, sulfate radical is just precipitated
Method is answered, by three sections of adverse current precipitation process, to realize the most of removing of sulfate radical in alkaline process production gallium electrolysis tail washings
Meanwhile, also generate unexpected technique effect can also be co-precipitated vanadium metal while precipitated sulfur acid group.
Specific embodiment
Embodiment：
The present invention, using a kind of barium salt for dissolving in strong base solution, just sinks under the solution system of highly basic to sulfate radical
Shallow lake method is answered, reaction condition：At 30-50 DEG C, the reaction time is 0.5-4 hours, mixing time 1-3 hours to temperature control；Sulfate radical
It is 1 with barium salt molal weight ratio：(0.8-1.4), sulfate radical and vanadium metal can be co-precipitated.In order that sulfate radical precipitation is more
Completely, barium salt can be utilized sufficiently, and precipitation operation is precipitated using multistage counter current, as a example by the present embodiment is precipitated from three sections of adverse currents
I.e. first paragraph precipitation process is precipitated using two sections of precipitating reagents that second segment precipitation process is obtained to new electrolysis tail washings, to obtain
Obtain one section of tail washings；
Second segment precipitation process is precipitated using one section of precipitating reagent to one section of tail washings；To obtain two sections of tail washings and two sections
Precipitating reagent；
3rd section of precipitation process is precipitated using new precipitating reagent to two sections of tail washings；To obtain qualified tail washings and second segment
One section of precipitating reagent needed for precipitation process.Above-mentioned new electrolysis tail washings is the initial tail washings after the completion of alkalescence production gallium, on
The new precipitating reagent stated is the precipitating reagent of just beginning and end and electrolysis tail washings.
Using the multistage counter current precipitation method, barium salt or alkali utilization rate can reach 80-90%, and sulfate radical can remove 90%,
While reaction precipitation reduction sulfate radical, vanadium metal is also co-precipitated.Vanadium metal can remove 90%.Test data is as follows：
In the description of this specification, the description of term " one embodiment " etc. means that combining the embodiment or example describes
Specific features, structure, material or feature be contained at least one embodiment of the invention or example.In this manual,
Schematic representation to above-mentioned term is not necessarily referring to identical embodiment or example.And, the specific features of description, knot
Structure, material or feature can in an appropriate manner be combined in one or more any embodiments or example.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (5)
1. the method that alkaline process produces gallium caustic alkali Recovery Purifying, it is characterised in that：By baric ion salt or the precipitation of alkali
Agent is added in new electrolyte, and the sulfate radical and the molal weight ratio of the barium ions in the new electrolysis tail washings are 1:(0.8-
1.4)。
2. the method that alkaline process according to claim 1 produces gallium caustic alkali Recovery Purifying, it is characterised in that：It is described heavy
Shallow lake agent is added to the new electrolysis tail washings using three sections of adverse current place of settling logos；
Wherein first paragraph precipitation process is precipitated using two sections of precipitating reagents that second segment precipitation process is obtained to new electrolysis tail washings,
To obtain one section of tail washings；
Second segment precipitation process is precipitated using one section of precipitating reagent to one section of tail washings；To obtain two sections of tail washings and two sections of precipitations
Agent；
3rd section of precipitation process is precipitated using new precipitating reagent to two sections of tail washings；To obtain qualified tail washings and second segment precipitation
One section of precipitating reagent needed for treatment.
3. the method that alkaline process according to claim 2 produces gallium caustic alkali Recovery Purifying, it is characterised in that：First paragraph
Precipitation process, second segment precipitation process and the 3rd section of precipitation process are carried out under conditions of being 30-50 DEG C in temperature.
4. the method that alkaline process according to claim 2 produces gallium caustic alkali Recovery Purifying, it is characterised in that：First paragraph
The reaction time of precipitation process, second segment precipitation process and the 3rd section of precipitation process is 0.5-4 hours.
5. the method that alkaline process according to claim 2 produces gallium caustic alkali Recovery Purifying, it is characterised in that：First paragraph
The precipitation mixing time of precipitation process, second segment precipitation process and the 3rd section of precipitation process is 1-3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611197219.0A CN106702429A (en) | 2016-12-22 | 2016-12-22 | Method for purifying and recovering caustic alkali for producing metal gallium through alkaline method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611197219.0A CN106702429A (en) | 2016-12-22 | 2016-12-22 | Method for purifying and recovering caustic alkali for producing metal gallium through alkaline method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106702429A true CN106702429A (en) | 2017-05-24 |
Family
ID=58938696
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611197219.0A Pending CN106702429A (en) | 2016-12-22 | 2016-12-22 | Method for purifying and recovering caustic alkali for producing metal gallium through alkaline method |
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Citations (14)
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|---|---|---|---|---|
| CN1186524A (en) * | 1995-06-07 | 1998-07-01 | 康明柯工程服务有限公司 | Chloride assisted hydrometallurgical extraction of nickel and cobalt from sulfide minerals |
| CN1271392A (en) * | 1997-08-15 | 2000-10-25 | 康明柯工程服务有限公司 | Chloride assisted hydrometallurgical extraction of nickel and cobalt fro m sulphide or laterite ores |
| CN1775972A (en) * | 2005-12-09 | 2006-05-24 | 韶关市华韦实业有限公司 | Technology for extracting Gallium metal from lead-zine tail ore slug smelting by extracting-electrolytic method |
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| CN102392137A (en) * | 2011-11-28 | 2012-03-28 | 太原工业学院 | Method for recovering silver from waste fixer by using acid as precipitant |
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| CN102560118A (en) * | 2012-01-09 | 2012-07-11 | 刘景洋 | Method for recycling tin and lead from waste circuit board leach liquor |
| CN103031450A (en) * | 2012-12-28 | 2013-04-10 | 北京吉亚半导体材料有限公司 | Purification method for gallium |
| CN103285628A (en) * | 2013-03-28 | 2013-09-11 | 卢普伦 | A sludge discharging inclined tube settling tank |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN104862503A (en) * | 2015-04-20 | 2015-08-26 | 中国恩菲工程技术有限公司 | Method for extracting scandium from nickel laterite ore |
| CN106011482A (en) * | 2016-06-30 | 2016-10-12 | 华南理工大学 | Chromium resource recycling and detoxification processing method for chromium slag |
| CN106086936A (en) * | 2016-08-31 | 2016-11-09 | 紫金铜业有限公司 | A kind of method of cleaning copper electrolyte remove impurity |
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-
2016
- 2016-12-22 CN CN201611197219.0A patent/CN106702429A/en active Pending
Patent Citations (14)
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| CN1186524A (en) * | 1995-06-07 | 1998-07-01 | 康明柯工程服务有限公司 | Chloride assisted hydrometallurgical extraction of nickel and cobalt from sulfide minerals |
| CN1271392A (en) * | 1997-08-15 | 2000-10-25 | 康明柯工程服务有限公司 | Chloride assisted hydrometallurgical extraction of nickel and cobalt fro m sulphide or laterite ores |
| CN1775972A (en) * | 2005-12-09 | 2006-05-24 | 韶关市华韦实业有限公司 | Technology for extracting Gallium metal from lead-zine tail ore slug smelting by extracting-electrolytic method |
| CN1818144A (en) * | 2005-12-22 | 2006-08-16 | 山东铝业股份有限公司 | Vanadium removal for electrolytic stoste in metal gallium electrolysis |
| CN102421514A (en) * | 2009-03-09 | 2012-04-18 | 阿文德·马立纳什·拉里 | Continuous countercurrent fluidized moving bed (fmb) and/or expanded moving bed (emb) |
| CN102392137A (en) * | 2011-11-28 | 2012-03-28 | 太原工业学院 | Method for recovering silver from waste fixer by using acid as precipitant |
| CN102560118A (en) * | 2012-01-09 | 2012-07-11 | 刘景洋 | Method for recycling tin and lead from waste circuit board leach liquor |
| CN103031450A (en) * | 2012-12-28 | 2013-04-10 | 北京吉亚半导体材料有限公司 | Purification method for gallium |
| CN103285628A (en) * | 2013-03-28 | 2013-09-11 | 卢普伦 | A sludge discharging inclined tube settling tank |
| CN103993331A (en) * | 2014-05-29 | 2014-08-20 | 珠海经济特区方源有限公司 | Method for treating gallium electrolysis tail liquid |
| CN104862503A (en) * | 2015-04-20 | 2015-08-26 | 中国恩菲工程技术有限公司 | Method for extracting scandium from nickel laterite ore |
| CN205687981U (en) * | 2016-06-23 | 2016-11-16 | 五矿（北京）稀土研究院有限公司 | A kind of for realizing fractional precipitation continuously and reclaiming the device of mother liquor of precipitation of ammonium |
| CN106011482A (en) * | 2016-06-30 | 2016-10-12 | 华南理工大学 | Chromium resource recycling and detoxification processing method for chromium slag |
| CN106086936A (en) * | 2016-08-31 | 2016-11-09 | 紫金铜业有限公司 | A kind of method of cleaning copper electrolyte remove impurity |
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Application publication date: 20170524 |