CN106435200A - Method for enriching as well as separating and recovering tellurium and bismuth from solution - Google Patents
Method for enriching as well as separating and recovering tellurium and bismuth from solution Download PDFInfo
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- CN106435200A CN106435200A CN201610813922.3A CN201610813922A CN106435200A CN 106435200 A CN106435200 A CN 106435200A CN 201610813922 A CN201610813922 A CN 201610813922A CN 106435200 A CN106435200 A CN 106435200A
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- tellurium
- bismuth
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- precipitation
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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
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
-
- 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
- C22B7/04—Working-up slag
-
- 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
Abstract
The invention discloses a method for enriching as well as separating and recovering tellurium and bismuth from a solution. A platinum and palladium sedimentation solution in anode mud treatment is used as a raw material and is treated by using a chemical method to realize the enriching as well as separation and recovery of tellurium and bismuth in the solution. The method comprises the steps of firstly, adding NaOH into the solution to regulate the pH value of the solution, and filtering to obtain tellurium and bismuth sediments; carrying out acid dissolution on the obtained tellurium and bismuth sediments, and filtering to obtain a tellurium and bismuth enriched leachate, wherein the leaching rate of tellurium reaches 98% or above, and the leaching rate of bismuth reaches 99% or above; directly reducing the tellurium and bismuth enriched leachate by using a reducing agent, and filtering to obtain tellurium powder and a tellurium reduction solution, wherein the reduction rate of tellurium reaches 99% or above; and adding an NaOH solution into the tellurium reduction solution, regulating the pH value of the solution, filtering to obtain bismuth oxychloride, adding the NaOH solution into the obtained bismuth oxychloride to regulate the pH value to dechlorinate, and filtering to obtain bismuth oxide.
Description
Technical field
The invention belongs to rare precious metal field of hydrometallurgy, and in particular to after the heavy platinum palladium after copper anode mud wet treatment in liquid
The concentration and separation recovery technology of tellurium bismuth, realizes the synthetical recovery of resource.
Background technology
Tellurium and its compound have numerous applications, and its application industry includes the every profession and trades such as light-sensitive material, refrigeration, solar energy, should
Directly determine the demand of tellurium with the state of development of industry.Cadmium telluride diaphragm solar industry development is rapid at present, it is considered to be
Most there is one of Application of Solar Energy technology of development potentiality, it is contemplated that as Cadimium telluride thin film is in the extensive application of solar energy industry, tellurium
Demand by continue growth go down.Bismuth has a lot of good characteristics, such as proportion is larger, fusing point is relatively low, solidification when volume occur
Expansion etc., among this, the avirulence of bismuth makes bismuth have numerous special purposes with safety.Being applied to metallurgy, change bismuth more
The various fields such as work.
Tellurium is mainly extracted recovery from copper, the nickel electrowinning earth of positive pole, while bismuth can be reclaimed.Copper, nickel electrowinning anode
Mud tellurium yield proportion is very big.Copper anode mud reclaims the precious metal solution that noble metal and noble metal purification process are produced, and becomes
Reclaim the another important sources of rare and scatter element bismuth tellurium.Bismuth is as a kind of little metal resource yield in the world all than relatively low.I
State's production bismuth is mainly refined from lead anode slurry, Copper making flue dust, pig iron smelting blast furnace dust and furnace bottom lead bismuth alloy and is obtained.From
In tellurobismuthite, separation and recovery tellurium bismuth leaches tellurobismuthite using acid and oxidant are compound at present, and leachate is reduced using sodium sulfite
To coarse tellurium powder obtain highly purified tellurium powder through pulping and washing.
The solution of noble metal gold, platinum, palladium and purification process generation is reclaimed in non-ferrous metal earth of positive pole hydrometallurgy, is typically contained
There are the metals such as a certain amount of gold, platinum, palladium, selenium, tellurium.Industrial main Au, Pt, Pd in reducing solution by the way of zinc dust precipitation
Deng rare precious metal, also containing elements such as larger amount of tellurium bismuths in the solution after reducing platinum palladium, separation and concentration is reclaimed therein
Bismuth tellurium.Traditional method for reclaiming tellurium bismuth from liquid after heavy platinum palladium obtains Na after typically precipitating by NaOH solution2TeO3Solution,
Na2TeO3Solution through repeated precipitation and alkali extraction pure after, electrolytic preparation simple substance tellurium.
The present invention mainly provides the technical method that a set of separation, impurity removal is enriched with tellurium bismuth.The method process is simple, recovery tellurium
Bismuth low cost, concentration effect are good, the response rate is high, be suitable for industrial demand, high-grade concentrate or product is obtained.
Content of the invention
The present invention is intended to provide a kind of succinct, efficient recovery metal process from solution, can make solution by the method
In bismuth metal and tellurium be enriched with reclaim.
The technical scheme is that：Liquid after heavy platinum palladium containing tellurium bismuth is poured in three-necked bottle, is added a certain amount of
NaOH solution at the same stirring and adjusting pH be 2～8, fully react after filter to obtain liquid after tellurium bismuth precipitation slag and precipitation tellurium bismuth.In tellurium bismuth
Add the mixed acid solution of hydrochloric acid or hydrochloric acid and sulphuric acid in precipitation slag, the acid of addition be with H+Densitometer, H+Concentration be 2mol/L～
6mol/L, liquid-solid ratio (mL:G) it is 3:1～8:1, the response time is that 0.5h～4h, reaction temperature is 10 DEG C～50 DEG C, adds mixed
When sour, Cl-Concentration control in 0.5mol/L～6mol/L, after fully reacting, the dissolution rate of bismuth reaches more than 99%, the dissolving of tellurium
Rate reaches more than 98% so that in leachate, the concentration of tellurium bismuth is significantly improved, and realizes the enrichment of tellurium bismuth.Leachate adopts SO2
Reduced, it is 0.5h～8h in 50 DEG C～95 DEG C, response time that reaction temperature is, reaction filter completely after tellurium powder and reductive tellurium
Liquid.
SO2The pH for adding sodium hydrate regulator solution after reductive tellurium in liquid is 1～5, and controlling reaction temperature is 10 DEG C～50
DEG C, response time 0.5h～4h, filters to obtain chlorine oxygen bismuth.Sodium hydroxide solution, concentration of sodium hydroxide solution is added in chlorine oxygen bismuth
For 4mol/L～8mol/L, liquid-solid ratio (mL:G) it is 3:1～8:1, response time 1h～4h, 60 DEG C～95 DEG C of reaction temperature, take off
Chlorine filters to obtain bismuth oxide completely afterwards, measures bismuth oxide purity through washing and drying and reaches 93.80%, reaches wanting for industrial refine
Ask.
Wherein, if the GOLD FROM PLATING SOLUTION owner's bismuth containing tellurium for processing in the technical scheme.
Beneficial effects of the present invention are as follows：
1) using hydrochloric acid or hydrochloric acid and sulphuric acid mixed acid solution by whole for tellurium bismuth precipitation slag dissolutions, leaching efficiency height, remove impurity
Effect is good, and tellurium bismuth obtains highly enriched, raising utilization rate of equipment and installations, reduces equipment investment；
2) using hydrochloric acid or hydrochloric acid and sulphuric acid mixed acid solution by whole for tellurium bismuth precipitation slag dissolutions, using SO2During reductive tellurium
Without the need for adding chloride ion again, make process simpler efficiently；Reduce production cost, with significant economic benefit；
3) this technology process is simple, in solution tellurium bismuth the response rate height, tellurium bismuth good separating effect, it is achieved that resource effective
Reclaim, substantially increase production efficiency.
Specific embodiment
Embodiment 1
Copper anode mud liquid 5L after the heavy platinum palladium that chlorination parting, zinc dust precipitation are obtained is taken, adds the NaOH solution of 5mol/L
Adjust pH=7, reaction 1 hour after, filter tellurium bismuth precipitation slag and precipitation tellurium bismuth after liquid.
Table 1-1 sink platinum palladium after liquid, precipitation tellurium bismuth after liquid, enrichment tellurium bismuth ammonium acetate/mgL-1
The tellurium bismuth precipitation slag 70.28g of above-mentioned drying is weighed, is put in the middle of three-necked bottle, by liquid-solid ratio (mL:G) it is 6:1
The hydrochloric acid 422mL for measuring 3mol/L pours startup stirring in the middle of three-necked bottle into, and reaction temperature is 50 DEG C, to react 2 hours, filters rich
The leachate of collection tellurium bismuth.After liquid after heavy platinum palladium, precipitation tellurium bismuth, its composition of leachate of liquid, enrichment tellurium bismuth is as shown in table 1-1.
The leachate 415mL of the enrichment tellurium bismuth obtained by measuring, pours in three-necked bottle and heats and start stirring, be passed through SO2,
Reaction under conditions of reaction temperature is 70 DEG C carries out 4h, and filtration washing is dried after obtaining 8.17 grams of tellurium powder and 400mL reductive tellurium
Liquid, after tellurium powder is dried, tellurium content reaches 83.77%, and the direct yield of tellurium reaches 97.63%.
Liquid composition/mgL after liquid after table 1-2 reductive tellurium, precipitation tellurium bismuth-1
Measure SO2After reductive tellurium, liquid 400mL is poured in three-necked bottle and is added NaOH solution to adjust pH=2, and the response time is 2h,
Reaction temperature is 50 DEG C carries out the precipitation experiments of bismuth, is filtrated to get liquid and precipitation slag chlorine oxygen bismuth after precipitated bismuth, liquid after its reductive tellurium,
After precipitated bismuth, liquid composition is as shown in table 1-2.
Concentration will be added in obtained chlorine oxygen bismuth for the sodium hydroxide solution of 6mol/L, liquid-solid ratio is 3:1, reaction temperature
During for 80 DEG C, filter after reaction 2h, washing and drying obtains 35.48 grams of solid bismuth oxide, and bi content reaches 74.60%,
The direct yield of bismuth reaches 94.83%.The composition of wherein chlorine oxygen bismuth, bismuth oxide is as shown in table 1-3.
Table 1-3 chlorine oxygen bismuth and bismuth oxide composition/%
Embodiment 2
Copper anode mud liquid 10L after the heavy platinum palladium that chlorination parting, zinc dust precipitation are obtained is taken, adds the NaOH solution of 5mol/L
Adjust pH=7.5, reaction 1 hour after, filter tellurium bismuth precipitation slag and precipitation tellurium bismuth after liquid.
Table 2-1 sink platinum palladium after liquid, precipitation tellurium bismuth after liquid, enrichment tellurium bismuth ammonium acetate/mgL-1
The precipitation slag 142.15g of bismuth containing tellurium of drying is weighed, is put in the middle of three-necked bottle, by liquid-solid ratio (mL:G) it is 6:1
The mixed acid solution for measuring 853mL is poured in the middle of three-necked bottle and starts stirring, nitration mixture be by the hydrochloric acid 600mL and 1.5mol/ of 3mol/L
The mix and blend of the sulphuric acid 300mL of L is obtained, and reaction temperature is 50 DEG C, to react 4 hours, filters the leachate that must be enriched with tellurium bismuth.Heavy
After liquid after platinum palladium, precipitation tellurium bismuth, its composition of leachate of liquid, enrichment tellurium bismuth is as shown in table 2-1.
The leachate 848mL of the enrichment tellurium bismuth obtained by measuring, pours in three-necked bottle and heats and start stirring, be passed through SO2,
Reaction under conditions of reaction temperature is 80 DEG C carries out 6h, filtration washing dry after 17.21 grams of tellurium powder and 840mL reductive tellurium
Liquid, after tellurium powder is dried, tellurium content reaches 79.66%, and the direct yield of tellurium reaches 97.79%.
Liquid composition/mgL after liquid after table 2-2 reductive tellurium, precipitation tellurium bismuth-1
Measure SO2After reductive tellurium, liquid 840mL is poured in three-necked bottle and is added NaOH solution to adjust pH=2, and the response time is 4h,
Reaction temperature is 50 DEG C carries out the precipitation experiments of bismuth, filters to obtain liquid and precipitation slag chlorine oxygen bismuth after precipitated bismuth, liquid after its reductive tellurium, heavy
After the bismuth of shallow lake, liquid composition is as shown in table 2-2.
Concentration will be added in obtained chlorine oxygen bismuth for the sodium hydroxide solution of 6mol/L, liquid-solid ratio is 3:1, reaction temperature
During for 80 DEG C, filter after reaction 4h, washing and drying obtains 71.15 grams of solid bismuth oxide, and bi content reaches 74.85%,
The direct yield of bismuth reaches 95.08%.The composition of wherein chlorine oxygen bismuth, bismuth oxide is as shown in table 2-3.
Table 2-3 chlorine oxygen bismuth and bismuth oxide composition/%
Embodiment 3
Copper anode mud liquid 50L after the heavy platinum palladium that chlorination parting, zinc dust precipitation are obtained is taken, adds the NaOH solution of 5mol/L
Adjust pH=7, reaction 1 hour after, filter tellurium bismuth precipitation slag and precipitation tellurium bismuth after liquid.
Table 3-1 sink platinum palladium after liquid, precipitation tellurium bismuth after liquid, enrichment tellurium bismuth ammonium acetate/mgL-1
The precipitation slag 712.25g of bismuth containing tellurium of drying is weighed, is put in the middle of three-necked bottle, by liquid-solid ratio (mL:G) it is 6:1
The mixed acid solution for measuring 4275.00mL is poured in the middle of three-necked bottle and starts stirring, nitration mixture be by the hydrochloric acid 3L and 1.5mol/ of 3mol/L
The mix and blend of the sulphuric acid 1.5L of L is obtained, and reaction temperature is 50 DEG C, to react 4 hours, filters the leachate that must be enriched with tellurium bismuth.Heavy
After liquid after platinum palladium, precipitation tellurium bismuth, its composition of leachate of liquid, enrichment tellurium bismuth is as shown in table 3-1.
The leachate 4270.00mL of the enrichment tellurium bismuth obtained by measuring, pours in three-necked bottle and heats and start stirring, be passed through
SO2, reaction under conditions of reaction temperature is 80 DEG C carries out 8h, filtration washing dry 85.41 grams of tellurium powder and 4260.00mL also
Liquid after former tellurium, after tellurium powder is dried, tellurium content reaches 80.42%, and the direct yield of tellurium reaches 97.99%.
Liquid composition/mgL after liquid after table 3-2 reductive tellurium, precipitation tellurium bismuth-1
Measure SO2After reductive tellurium, liquid 4260.00mL is poured in three-necked bottle and is added NaOH solution to adjust pH=2, response time
For 4h, reaction temperature is 50 DEG C carries out the precipitation experiments of bismuth, filters to obtain liquid and precipitation slag chlorine oxygen bismuth after precipitated bismuth, after its reductive tellurium
After liquid, precipitated bismuth, liquid composition is as shown in table 3-2.
Concentration will be added in obtained chlorine oxygen bismuth for the sodium hydroxide solution of 6mol/L, liquid-solid ratio is 3:1, reaction temperature
During for 80 DEG C, filter after reaction 4h, washing and drying obtains 358.40 grams of solid bismuth oxide, and bi content reaches 74.80%, bismuth
Direct yield reach 95.27%.The composition of wherein chlorine oxygen bismuth, bismuth oxide is as shown in table 3-3.
Table 3-3 chlorine oxygen bismuth and bismuth oxide composition/%
Claims (4)
1. a kind of method of enrichment and separation and recovery tellurium bismuth from solution, its feature comprises the steps of：
The pH for adding sodium hydrate regulator solution in the solution containing tellurium bismuth is 2～8, filters to obtain tellurium bismuth precipitation slag and precipitation tellurium bismuth
Liquid, adds hydrochloric acid or nitration mixture so that precipitation slag is fully dissolved in the precipitation slag of tellurium bismuth afterwards, when adding nitration mixture, Cl-Concentration control
In 0.5mol/L ~ 6mol/L, the leachate that must be enriched with tellurium bismuth is filtered, toward in the leachate of enrichment tellurium bismuth, be passed through SO2Reductive tellurium, mistake
Filter obtains liquid after tellurium powder and reductive tellurium, and the pH for adding sodium hydrate regulator solution after reductive tellurium in liquid is 1～5 precipitated bismuth, mistake
Filter obtains chlorine oxygen bismuth, adds concentration for the sodium hydroxide solution of 4mol/L ~ 8mol/L, filter and must aoxidize after reaction in chlorine oxygen bismuth
Bismuth.
2. according to claim 1 a kind of from solution enrichment with separation and recovery tellurium bismuth method, it is characterised in that：In tellurium
The hydrochloric acid for adding in the precipitation slag of bismuth or nitration mixture, the nitration mixture is the mixed acid solution of hydrochloric acid and sulphuric acid, the acid of addition be with H+Dense
Degree meter, H+Concentration is 2mol/L ~ 6mol/L, and acid is 3 with the liquid-solid ratio of precipitation slag:1~8:1, unit for ml/g, the response time
For 0.5 ~ 4h, reaction temperature is 10 DEG C ~ 50 DEG C, when adding nitration mixture, Cl-Concentration control in 0.5mol/L ~ 5mol/L.
3. according to claim 1 a kind of from solution enrichment with separation and recovery tellurium bismuth method, it is characterised in that：It is passed through
SO2Reductive tellurium, it is 0.5h ~ 8h in 50 DEG C ~ 95 DEG C, response time that reaction temperature is, reaction filter completely after tellurium powder and reductive tellurium
Liquid.
4. according to claim 1 a kind of from solution enrichment with separation and recovery tellurium bismuth method, it is characterised in that：Reduction
The pH for adding sodium hydrate regulator solution after tellurium in liquid is 1 ~ 5, controlling reaction temperature at 10 DEG C ~ 50 DEG C, response time 0.5h ~
4h, obtains chlorine oxygen bismuth, adds sodium hydroxide solution in chlorine oxygen bismuth, and concentration of sodium hydroxide solution is that 4mol/L ~ 8mol/L, liquid is solid
Than for 3:1~8:1, unit is mL/g, response time 1h ~ 6h, 60 DEG C ~ 95 DEG C of reaction temperature, obtains bismuth oxide after reaction completely.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107034358A (en) * | 2017-04-27 | 2017-08-11 | 中南大学 | A kind of reductive hydrolysis Enrichment and the method for reclaiming Au, Pt, Pd selen-tellurjum bismuth |
| CN107142377A (en) * | 2017-04-27 | 2017-09-08 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN107746956A (en) * | 2017-11-03 | 2018-03-02 | 郴州兴城环保股份有限公司 | Using the technique of support methods recovery tellurium from complicated solution |
| CN109402392A (en) * | 2018-09-11 | 2019-03-01 | 江西铜业股份有限公司 | A method of extracting tellurium from copper anode mud |
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| CN101338368A (en) * | 2008-08-08 | 2009-01-07 | 中南大学 | Method for preprocessing anode sludge and recovering dissipated metal |
| JP2015113267A (en) * | 2013-12-13 | 2015-06-22 | 三菱マテリアル株式会社 | Separation/recovery method of tellurium |
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| CN101289171A (en) * | 2008-06-02 | 2008-10-22 | 王钧 | Hydrometallurgy process for abstracting 99.99146004050f Te and 99.9926340320f Bi2O3 and comprehensively recovering accessory products |
| CN101338368A (en) * | 2008-08-08 | 2009-01-07 | 中南大学 | Method for preprocessing anode sludge and recovering dissipated metal |
| JP2015113267A (en) * | 2013-12-13 | 2015-06-22 | 三菱マテリアル株式会社 | Separation/recovery method of tellurium |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107034358A (en) * | 2017-04-27 | 2017-08-11 | 中南大学 | A kind of reductive hydrolysis Enrichment and the method for reclaiming Au, Pt, Pd selen-tellurjum bismuth |
| CN107142377A (en) * | 2017-04-27 | 2017-09-08 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN107142377B (en) * | 2017-04-27 | 2018-12-21 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN107746956A (en) * | 2017-11-03 | 2018-03-02 | 郴州兴城环保股份有限公司 | Using the technique of support methods recovery tellurium from complicated solution |
| CN107746956B (en) * | 2017-11-03 | 2019-05-28 | 郴州兴城环保股份有限公司 | Using the technique of support methods recycling tellurium from complicated solution |
| CN109402392A (en) * | 2018-09-11 | 2019-03-01 | 江西铜业股份有限公司 | A method of extracting tellurium from copper anode mud |
| CN109402392B (en) * | 2018-09-11 | 2020-05-12 | 江西铜业股份有限公司 | Method for extracting tellurium from copper anode slime |
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Application publication date: 20170222 |