CN110482496A - A method of recycling tellurium from Pt Pd concentrate - Google Patents
A method of recycling tellurium from Pt Pd concentrate Download PDFInfo
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- CN110482496A CN110482496A CN201910887251.9A CN201910887251A CN110482496A CN 110482496 A CN110482496 A CN 110482496A CN 201910887251 A CN201910887251 A CN 201910887251A CN 110482496 A CN110482496 A CN 110482496A
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- 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
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The method that the invention discloses a kind of to recycle tellurium from Pt Pd concentrate.Water slurry is added in Pt Pd concentrate, hydrochloric acid then is added and then hydrogen peroxide, pyroreaction filter, obtains filtrate and filter residue；It puts the filtrate into sealing reaction kettle, temperature is 170-180 DEG C, pressure is to stir 2-4h under 3-5 atmospheric pressure, then cooled and filtered, obtains H2TeO4Powder and filtrate；The H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 250-320 DEG C, and calcination time 4-5h obtains tellurium dioxide；Tellurium dioxide is subjected to alkaline leaching, alkaline leaching liquid is obtained, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtains tellurium piece, tellurium piece obtains Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting.Present invention process is simple, and process is short, and the tellurium ingot that purity is higher than 99.99% can be obtained in the rate of recovery and recycling purity is high of tellurium.
Description
Technical field
The method that the present invention relates to a kind of to recycle tellurium from Pt Pd concentrate, belongs to comprehensive utilization of waste technical field.
Background technique
Tellurium is the crystallization of orthorhombic system silvery white.Vitriolization, nitric acid, chloroazotic acid, potassium cyanide, potassium hydroxide；Insoluble in cold water
With hot water, carbon disulfide.Using tellurium powder as raw material, purification being extracted with sodium polysulfide and is obtained, it is 99.999% that high purity tellurium purity, which is made,.
For semiconductor devices,Alloy, industrial chemicals andCast iron、Rubber、GlassAdditive is used as in equal industry.
There are two types of telluriumsAllotrope, i.e. black powder, amorphous tellurium and silvery white, metallic luster, hexagonal crystal system
Crystalline state tellurium semiconductor, wide 0.34 electron volts of forbidden band.
In two kinds of allotropes of tellurium, one isCrystalTellurium, have metallic luster, silvery white, property is crisp, is and antimony phase
As；Another kind is amorphous powder, is in dark gray.Density is medium, melt, boiling point it is lower.It is a kind of nonmetalloid, can
It but has very good heat transfer and conducting power.In all nonmetallic companions, itMetallicityIt is strongest.
With the development of the social economy, the demand to tellurium is growing day by day.Copper anode mud is comprehensive to extract rare precious metal process
In, be added into liquid after turmeric after zinc dust precipitation platinum palladium and add piece alkali neutralization and obtain Pt Pd concentrate, in Pt Pd concentrate containing gold,
The rare precious metals such as platinum, palladium, tellurium.The generally about 5-20% containing tellurium, tellurium are usually deposited in the form of tellurium dioxide, tellurium simple substance in Pt Pd concentrate
In.The method that therefore, it is necessary to a kind of to recycle tellurium from Pt Pd concentrate.
Summary of the invention
In view of this, the method that the present invention provides a kind of to recycle tellurium from Pt Pd concentrate, simple process, process is short, tellurium
The rate of recovery and recycling purity is high, can be obtained purity be higher than 99.99% tellurium ingot.
The present invention solves above-mentioned technical problem by following technological means:
A kind of method recycling tellurium from Pt Pd concentrate of the invention, is following steps:
1) water slurry is added in Pt Pd concentrate, hydrochloric acid and hydrogen peroxide is then added, be 90-100 DEG C of reaction 1-2h in temperature,
Then it filters, obtains filtrate and filter residue；
2) it puts the filtrate into sealing reaction kettle, temperature is 170-180 DEG C, pressure is to stir 2- under 3-5 atmospheric pressure
4h is subsequently cooled to filter after temperature is 40-60 DEG C, obtains H2TeO4Powder and filtrate；
3) H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 250-320 DEG C, calcining
Time is 4-5h, obtains tellurium dioxide；
4) tellurium dioxide is subjected to alkaline leaching, obtains alkaline leaching liquid, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtain
Tellurium piece, tellurium piece obtain Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting.
The mass ratio 1:2-3 of Pt Pd concentrate and water in the step (1) is added hydrochloric acid and makes the concentration of hydrochloric acid in slurry to be
2-4mol/L, the molal quantity of the hydrogen peroxide of addition are 4-5 times of tellurium molal quantity.
H is obtained in the step (2)2TeO4Powder stops after pure water to conductivity≤100 μ S/cm of washing water is added
It only washs, washing water return step (1) pulp Pt Pd concentrate.
Gas obtained in the step (3) is absorbed liquid after sodium hydroxide absorbs, and absorbing liquid is put into sealing
Sulfuric acid is added in container, obtained gas returns after water removal and H2TeO4Powder metallurgy calcining, remaining solution is by concentration
Crystallization obtains sodium sulfate crystal.
Step (4) neutral and alkali, which leaches, uses sodium hydroxide solution, concentration 220-250g/L, and extraction temperature is
95-98 DEG C, extraction time 2-3h, the mass ratio of sodium hydroxide solution and tellurium dioxide is 2-4:1.
The electrodeposition process of tellurium in the step (4) are as follows: current density 150-220A/m2, tank voltage 2.5-5V, anode
Plate and cathode plate are respectively titanium plate and stainless steel plate, plate spacing 5-10cm.
The Te9999 trade mark tellurium ingot that the step (4) obtains meets " YST 222-2010 tellurium ingot " standard.
The present invention dissolves the tellurium in Pt Pd concentrate using oxidant is added in acid condition, obtains solution containing tellurium, so
After filter, hydro-thermal reaction occurs at high temperature for obtained filtrate, obtains H not soluble in water2TeO4Powder can be with using this technique
It is higher containing telloy to obtain purity, to realize tellurium and other impurities, such as the separation of copper, nickel, this technological operation is simple,
Process is short, and the precipitating purity is high and the rate of recovery of obtained tellurium are high；
Then high-temperature calcination is carried out under sulfur dioxide atmosphere again, under weak reducing atmosphere, H2TeO4It has been reduced into dioxy
Change tellurium, using this reducing process, can avoid introducing impurity, so that it is very high to obtain purity to avoid being restored in the liquid phase
Tellurium dioxide powder；
Liquid alkaline reaction is added in tellurium dioxide, obtained solution obtains tellurium piece by electrodeposition, then obtains by ingot casting pure
Spend the tellurium ingot of > 99.99%.
Beneficial effects of the present invention: simple process, process is short, and purity is high can be obtained in the rate of recovery and recycling purity is high of tellurium
In 99.99% tellurium ingot.
Detailed description of the invention
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is 1H of the embodiment of the present invention2TeO4The SEM of powder.
Fig. 2 is 2H of the embodiment of the present invention2TeO4The SEM of powder.
Fig. 3 is the SEM of 1 tellurium dioxide of the embodiment of the present invention.
Fig. 4 is the SEM of 2 tellurium dioxide of the embodiment of the present invention.
Specific embodiment
Below with reference to attached drawing, the present invention is described in detail, and a kind of of the present embodiment recycles tellurium from Pt Pd concentrate
Method is following steps:
1) water slurry is added in Pt Pd concentrate, hydrochloric acid and hydrogen peroxide is then added, be 90-100 DEG C of reaction 1-2h in temperature,
Then it filters, obtains filtrate and filter residue；
2) it puts the filtrate into sealing reaction kettle, temperature is 170-180 DEG C, pressure is to stir 2- under 3-5 atmospheric pressure
4h is subsequently cooled to filter after temperature is 40-60 DEG C, obtains H2TeO4Powder and filtrate；
3) H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 250-320 DEG C, calcining
Time is 4-5h, obtains tellurium dioxide；
4) tellurium dioxide is subjected to alkaline leaching, obtains alkaline leaching liquid, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtain
Tellurium piece, tellurium piece obtain Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting.
The mass ratio 1:2-3 of Pt Pd concentrate and water in the step (1) is added hydrochloric acid and makes the concentration of hydrochloric acid in slurry to be
2-4mol/L, the molal quantity of the hydrogen peroxide of addition are 4-5 times of tellurium molal quantity.
H is obtained in the step (2)2TeO4Powder stops after pure water to conductivity≤100 μ S/cm of washing water is added
It only washs, washing water return step (1) pulp Pt Pd concentrate.
Gas obtained in the step (3) is absorbed liquid after sodium hydroxide absorbs, and absorbing liquid is put into sealing
Sulfuric acid is added in container, obtained gas returns after water removal and H2TeO4Powder metallurgy calcining, remaining solution is by concentration
Crystallization obtains sodium sulfate crystal.
Step (4) neutral and alkali, which leaches, uses sodium hydroxide solution, concentration 220-250g/L, and extraction temperature is
95-98 DEG C, extraction time 2-3h, the mass ratio of sodium hydroxide solution and tellurium dioxide is 2-4:1.
The electrodeposition process of tellurium in the step (4) are as follows: current density 150-220A/m2, tank voltage 2.5-5V, anode
Plate and cathode plate are respectively titanium plate and stainless steel plate, plate spacing 5-10cm.
The Te9999 trade mark tellurium ingot that the step (4) obtains meets " YST 222-2010 tellurium ingot " standard.
Embodiment 1
A method of it recycling tellurium from Pt Pd concentrate, is following steps:
1) Pt Pd concentrate is taken, testing result is as follows:
It is added into water slurry, hydrochloric acid and hydrogen peroxide is then added, salt is added in the mass ratio 1:2.7 of Pt Pd concentrate and water
Acid makes the concentration of hydrochloric acid in slurry be 3mol/L, and the molal quantity of the hydrogen peroxide of addition is that 4.7 times of tellurium molal quantity are in temperature
98 DEG C of reaction 1.5h, then filter, obtain filtrate and filter residue, obtained filtrate testing result is as follows:
2) it puts the filtrate into sealing reaction kettle, temperature is 175 DEG C, pressure is to stir 3h under 3.2 atmospheric pressure, then
It is cooled to after temperature is 55 DEG C and filters, obtain H2TeO4Powder and filtrate, obtain H2TeO4Pure water is added to washing water in powder
Conductivity≤100 μ S/cm after stop washing, washing water return step (1) pulp Pt Pd concentrate, obtained H2TeO4Powder inspection
Measured data is as follows:
| Element | Te | Pt | Pd | Cu | Ni | Sn | Au |
| Content | 65.33% | 0.1ppm | 0.1ppm | 0.9ppm | 2.1ppm | 1.1ppm | 0.1ppm |
| Ca | Fe | Mg | Bi | Pb | Co | Mn | Zn |
| 0.4ppm | 1.2ppm | 3.2ppm | 2.4ppm | 0.7ppm | 2.1ppm | 6.5ppm | 3.5ppm |
As shown in Figure 1, obtained H2TeO4Powder is in granular form.
3) H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 250-320 DEG C, calcining
Time is 4-5h, obtains tellurium dioxide, and obtained gas is absorbed liquid after sodium hydroxide absorbs, and absorbing liquid is put into close
Sulfuric acid is added in envelope container, obtained gas returns after water removal and H2TeO4Powder metallurgy calcining, remaining solution is through overrich
Sheepshank crystalline substance obtains sodium sulfate crystal, and the detection data of obtained tellurium dioxide is as follows:
| Element | Te | Pt | Pd | Cu | Ni | Sn | Au |
| Content | 79.41% | 0.13ppm | 0.15ppm | 2.12ppm | 3.25ppm | 1.12ppm | 0.1ppm |
| Ca | Fe | Mg | Bi | Pb | Co | Mn | Zn |
| 0.43ppm | 2.1ppm | 4.2ppm | 2.9ppm | 1.1ppm | 2.9ppm | 8.9ppm | 5.4ppm |
As shown in figure 3, obtained tellurium dioxide graininess spherical in shape, partial size are small.
4) tellurium dioxide is subjected to alkaline leaching, obtains alkaline leaching liquid, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtain
Tellurium piece, tellurium piece obtain Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting；
Alkaline leaching uses sodium hydroxide solution, concentration 235g/L, and extraction temperature is 96 DEG C, and extraction time is
The mass ratio of 2.5h, sodium hydroxide solution and tellurium dioxide is 3:1.
The electrodeposition process of tellurium in the step (4) are as follows: current density 185A/m2, tank voltage 2.9V, anode plate and yin
Pole plate is respectively titanium plate and stainless steel plate, plate spacing 8cm.
The Te9999 trade mark tellurium ingot that the step (4) obtains meets " YST 222-2010 tellurium ingot " standard.
The comprehensive recovery of final the present embodiment tellurium reaches 98.7%.
Embodiment 2
A method of it recycling tellurium from Pt Pd concentrate, is following steps:
1) water slurry is added in Pt Pd concentrate, hydrochloric acid and hydrogen peroxide is then added, be 99 DEG C of reaction 2h in temperature, then mistake
Filter, obtains filtrate and filter residue；
2) it puts the filtrate into sealing reaction kettle, it is then cold temperature is 178 DEG C, pressure is to stir 3h under 4 atmospheric pressure
But it is filtered after being 55 DEG C to temperature, obtains H2TeO4Powder and filtrate；
3) H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 310 DEG C, calcination time
For 4.5h, tellurium dioxide is obtained；
4) tellurium dioxide is subjected to alkaline leaching, obtains alkaline leaching liquid, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtain
Tellurium piece, tellurium piece obtain Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting.
The mass ratio 1:3 of Pt Pd concentrate and water in the step (1) is added hydrochloric acid and makes the concentration of hydrochloric acid in slurry to be
3.5mol/L, the molal quantity of the hydrogen peroxide of addition are 5 times of tellurium molal quantity.
H is obtained in the step (2)2TeO4Powder stops after pure water to conductivity≤100 μ S/cm of washing water is added
It only washs, washing water return step (1) pulp Pt Pd concentrate.
Gas obtained in the step (3) is absorbed liquid after sodium hydroxide absorbs, and absorbing liquid is put into sealing
Sulfuric acid is added in container, obtained gas returns after water removal and H2TeO4Powder metallurgy calcining, remaining solution is by concentration
Crystallization obtains sodium sulfate crystal.
Step (4) neutral and alkali, which leaches, uses sodium hydroxide solution, concentration 245g/L, and extraction temperature is 96 DEG C,
Extraction time is 3h, and the mass ratio of sodium hydroxide solution and tellurium dioxide is 3.5:1.
The electrodeposition process of tellurium in the step (4) are as follows: current density 210A/m2, tank voltage 3.5V, anode plate and yin
Pole plate is respectively titanium plate and stainless steel plate, plate spacing 8cm.
The Te9999 trade mark tellurium ingot that the step (4) obtains meets " YST 222-2010 tellurium ingot " standard.
As shown in Fig. 2, obtained H2TeO4Powder is in granular form, and this nutty structure facilitates and washed, such as Fig. 4 institute
Show, obtained tellurium dioxide obtains graininess spherical in shape, and partial size is small, and single crystal grain is in 200nm or so, it may be convenient to carry out alkali soluble
Solution.
The comprehensive recovery of the present embodiment tellurium reaches 99.1%.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (7)
1. a kind of method for recycling tellurium from Pt Pd concentrate, which is characterized in that be following steps:
1) water slurry is added in Pt Pd concentrate, hydrochloric acid and hydrogen peroxide is then added, be 90-100 DEG C of reaction 1-2h in temperature, then
Filtering, obtains filtrate and filter residue；
2) it puts the filtrate into sealing reaction kettle, temperature is 170-180 DEG C, pressure is to stir 2-4h under 3-5 atmospheric pressure, so
After be cooled to temperature be 40-60 DEG C after filter, obtain H2TeO4Powder and filtrate；
3) H that will be obtained2TeO4Powder is calcined in sulfur dioxide air-flow high temperature, and calcination temperature is 250-320 DEG C, calcination time
For 4-5h, tellurium dioxide is obtained；
4) tellurium dioxide is subjected to alkaline leaching, obtains alkaline leaching liquid, carries out electrodeposition after the removal of impurities of alkaline leaching liquid, obtain tellurium
Piece, tellurium piece obtain Te9999 trade mark tellurium ingot by hot pure water washing, drying, ingot casting.
2. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (1)
The mass ratio 1:2-3 of middle Pt Pd concentrate and water is added hydrochloric acid and the concentration of hydrochloric acid in slurry is made to be 2-4mol/L, the dioxygen of addition
The molal quantity of water is 4-5 times of tellurium molal quantity.
3. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (2)
In obtain H2TeO4Powder stops washing after pure water to conductivity≤100 μ S/cm of washing water is added, and washing water returns to step
Suddenly (1) pulp Pt Pd concentrate.
4. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (3)
Obtained in gas be absorbed after sodium hydroxide absorbs liquid, absorbing liquid is put into sealing container, sulfuric acid is added, obtained
Gas by water removal after return and H2TeO4Powder metallurgy calcining, remaining solution obtain sodium sulfate crystal by condensing crystallizing.
5. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (4)
Neutral and alkali, which leaches, uses sodium hydroxide solution, concentration 220-250g/L, and extraction temperature is 95-98 DEG C, extraction time 2-
The mass ratio of 3h, sodium hydroxide solution and tellurium dioxide is 2-4:1.
6. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (4)
The electrodeposition process of middle tellurium are as follows: current density 150-220A/m2, tank voltage 2.5-5V, anode plate and cathode plate are respectively titanium
Plate and stainless steel plate, plate spacing 5-10cm.
7. a kind of method for recycling tellurium from Pt Pd concentrate according to claim 1, it is characterised in that: the step (4)
Obtained Te9999 trade mark tellurium ingot meets " YST 222-2010 tellurium ingot " standard.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112609089A (en) * | 2021-01-11 | 2021-04-06 | 大冶有色金属有限责任公司 | Method for enriching tellurium from platinum-palladium concentrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045849A (en) * | 2012-12-19 | 2013-04-17 | 江西铜业股份有限公司 | Pretreatment method for platinum palladium concentrate |
| CN104762471A (en) * | 2015-04-27 | 2015-07-08 | 中南大学 | Method for tellurium residue enhanced leaching |
| CN105905874A (en) * | 2016-04-19 | 2016-08-31 | 浙江亚栋实业有限公司 | Method of recycling tellurium from anode mud |
| CN106381399A (en) * | 2016-09-27 | 2017-02-08 | 郴州市金贵银业股份有限公司 | Method for recovering tellurium from high-tellurium residues |
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- 2019-09-19 CN CN201910887251.9A patent/CN110482496B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045849A (en) * | 2012-12-19 | 2013-04-17 | 江西铜业股份有限公司 | Pretreatment method for platinum palladium concentrate |
| CN104762471A (en) * | 2015-04-27 | 2015-07-08 | 中南大学 | Method for tellurium residue enhanced leaching |
| CN105905874A (en) * | 2016-04-19 | 2016-08-31 | 浙江亚栋实业有限公司 | Method of recycling tellurium from anode mud |
| CN106381399A (en) * | 2016-09-27 | 2017-02-08 | 郴州市金贵银业股份有限公司 | Method for recovering tellurium from high-tellurium residues |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112609089A (en) * | 2021-01-11 | 2021-04-06 | 大冶有色金属有限责任公司 | Method for enriching tellurium from platinum-palladium concentrate |
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