CN105271137B - A kind of method that tellurium dioxide is extracted in the copper ashes from telluride - Google Patents
A kind of method that tellurium dioxide is extracted in the copper ashes from telluride Download PDFInfo
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- CN105271137B CN105271137B CN201510797529.5A CN201510797529A CN105271137B CN 105271137 B CN105271137 B CN 105271137B CN 201510797529 A CN201510797529 A CN 201510797529A CN 105271137 B CN105271137 B CN 105271137B
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- tellurium
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- reaction
- telluride
- copper ashes
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 24
- 239000010949 copper Substances 0.000 title claims abstract description 24
- 235000002918 Fraxinus excelsior Nutrition 0.000 title claims abstract description 23
- 239000002956 ash Substances 0.000 title claims abstract description 23
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 25
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 25
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000007788 liquid Substances 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 238000002386 leaching Methods 0.000 claims description 25
- 239000003513 alkali Substances 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 239000002893 slag Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 10
- 235000021110 pickles Nutrition 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000013589 supplement Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- QZCHKAUWIRYEGK-UHFFFAOYSA-N tellanylidenecopper Chemical compound [Te]=[Cu] QZCHKAUWIRYEGK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention provides a kind of method that tellurium dioxide is extracted in copper ashes from telluride, and pure tellurium dioxide powder is obtained using the method for the heavy tellurium-salt Ore Leaching-secondary neutralization of alkaline pressure of oxygen leaching-neutralization；The present invention can efficiently extract the tellurium metal in telluride copper ashes, and investment is less, and easy to operate, energy resource consumption is less, simple production process, and the rate of recovery of tellurium is up to more than 90%.
Description
Technical field
The invention belongs to metallurgical technology field, and in particular to a kind of method that tellurium dioxide is extracted in copper ashes from telluride.
Background technology
The main source of tellurium is copper anode mud, and in wet-treating copper anode mud, the tellurium for having 40% ~ 60% enters pickle liquor,
Reclaimed using copper powder reduction, obtain copper tellurium slag.At present, the conventional method for handling copper tellurium slag is：Copper tellurium slag roasts through sulphation
After burning, alkali leaching divides tellurium, finally the purified treatment recovery metallic tellurium by series, and its shortcoming is that a large amount of sulfuric acid are admixed in raw material, roasting
Needed after burning by ball milling, then substantial amounts of alkali is consumed during alkali leaching, build environment is poor, and complex manufacturing, flow is longer, tellurium recovery
Rate is low.
The content of the invention
The defects of for prior art, the present invention provide a kind of method that tellurium dioxide is extracted in copper ashes from telluride.
The technical scheme is that：A kind of method that tellurium dioxide is extracted in copper ashes from telluride, comprises the following steps：
Step（1）Alkaline pressure of oxygen leaching：By solid-liquid mass ratio 1:5~7 sodium hydroxide solution and telluride by concentration for 150g/L
Copper ashes is well mixed, and is placed in autoclave, is added vulcanized sodium, is heated to 130 ~ 140 DEG C, is led to oxygen to 0.6 ~ 0.7Mpa, is kept
3 ~ 4h of pressure, filtered after being cooled to 50 ~ 60 DEG C, the recovery of alkali phase analysis, alkali soaks again；
Step（2）Neutralize heavy tellurium：To step（1）The sulfuric acid that concentration is 4mol/L is added in gained alkali immersion liquid, adjusts pH to 4
~5, for heating response liquid to 80 ~ 90 DEG C, the reaction time is 1 ~ 2h, supplements sulfuric acid during reaction, pH value of solution is maintained 4.5 ~ 5,
At the end of reaction, pH terminals are 4.5~5, and reaction solution is cooled to 50~60 DEG C, filters while hot, is washed to neutrality, liquid after must neutralizing
With neutralization slag, liquid reclaims after neutralization；
Step（3）Salt Ore Leaching：By step（2）Neutralization slag after cleaning is put into 6mol/L hydrochloric acid, controls solid-liquid matter
Amount is than being 1:6~7, heating response temperature is 75~85 DEG C, stirs 2 ~ 3h；Chilling temperature obtains acidleach to filtering after 50~60 DEG C
Liquid and sour slag, sour slag continue alkali leaching after telluride copper ashes is included into after stacking and drying；
Step（4）Secondary neutralization：By step（3）The secondary neutralization of gained pickle liquor sodium hydroxide, pH to 5~6 is adjusted, is added
For thermal response liquid to 80~90 DEG C, the reaction time is 1 ~ 2h, and sodium hydroxide is supplemented during reaction, and at the end of reaction, pH terminals are 5.5
~6, reaction solution is cooled to 50~60 DEG C, filtering, is washed to neutrality, obtains pure tellurium dioxide powder.
Beneficial effects of the present invention are：The tellurium metal in telluride copper ashes can be efficiently extracted, invests less, operation side
Just, energy resource consumption is less, simple production process, and the rate of recovery of tellurium is up to more than 90%.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
With reference to Fig. 1 and specific embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of method that tellurium dioxide is extracted in copper ashes from telluride, comprises the following steps：
Step（1）Alkaline pressure of oxygen leaching：By solid-liquid mass ratio 1:5 sodium hydroxide solution and telluride copper ashes by concentration for 150g/L
It is well mixed, it is placed in autoclave, adds appropriate vulcanized sodium, be heated to 130 DEG C, leads to oxygen to 0.6Mpa, keep pressure 3h, treat
Filtered after being cooled to 50 DEG C, the recovery of alkali phase analysis, alkali soaks again, and the leaching rate of tellurium is 95.7% after alkali soaks；
Step（2）Neutralize heavy tellurium：To step（1）In gained alkali immersion liquid add concentration be 4mol/L sulfuric acid, regulation pH to
4, heating response liquid reaction time 1h, sulfuric acid is supplemented during reaction to 80 DEG C, pH value of solution is maintained 4.5, reaction terminates
When, pH terminals are 4.5, and reaction solution is cooled to 50 DEG C, filters while hot, is washed to neutrality, liquid and neutralization slag after must neutralizing, after neutralization
Liquid reclaims, and the yield of tellurium is 99.5%；
Step（3）Salt Ore Leaching：By step（2）Neutralization slag after cleaning is put into 6mol/L hydrochloric acid, controls solid-liquid matter
Amount is than being 1:6, heating response temperature is 75 DEG C, stirs 2h；Chilling temperature obtains pickle liquor and sour slag to filtering after 50 DEG C, acid
Slag continues alkali leaching after telluride copper ashes is included into after stacking and drying, and the direct yield of the tellurium of hydrochloric acid leaching process is 90.87%；
Step（4）Secondary neutralization：By step（3）The secondary neutralization of gained pickle liquor sodium hydroxide, adjust pH to 5, heating
Reaction solution reaction time 1h, supplements sodium hydroxide to 80 DEG C during reaction, at the end of reaction, pH terminals are 5.5, reaction solution
50 DEG C are cooled to, filtering, is washed to neutrality, obtains pure tellurium dioxide powder, the direct yield of tellurium is 99.7%.
Embodiment 2
A kind of method that tellurium dioxide is extracted in copper ashes from telluride, comprises the following steps：
Step（1）Alkaline pressure of oxygen leaching：By solid-liquid mass ratio 1:6 sodium hydroxide solution and telluride copper ashes by concentration for 150g/L
It is well mixed, it is placed in autoclave, adds appropriate vulcanized sodium, be heated to 135 DEG C, leads to oxygen to 0.65Mpa, keep pressure
3.5h, filtered after being cooled to 55 DEG C, the recovery of alkali phase analysis, alkali soaks again, and the leaching rate of tellurium is 94.6%；
Step（2）Neutralize heavy tellurium：To step（1）In gained alkali immersion liquid add concentration be 4mol/L sulfuric acid, regulation pH to
4.5, heating response liquid reaction time 1.5h, sulfuric acid is supplemented during reaction to 85 DEG C, pH value of solution is maintained 4.8, reaction knot
Shu Shi, pH terminal are 4.8, and reaction solution is cooled to 55 DEG C, filters while hot, is washed to neutrality, and liquid and neutralization slag, are neutralized after must neutralizing
Liquid reclaims afterwards, and the yield of tellurium is 99.3%；
Step（3）Salt Ore Leaching：By step（2）Neutralization slag after cleaning is put into 6mol/L hydrochloric acid, controls solid-liquid matter
Amount is than being 1:6.5, heating response temperature is 80 DEG C, stirs 2.5h；Chilling temperature obtains pickle liquor and acid is molten to filtering after 55 DEG C
Slag, sour slag continue alkali leaching after telluride copper ashes is included into after stacking and drying, and the leaching rate of hydrochloric acid leaching process is 90.1%；
Step（4）Secondary neutralization：By step（3）The secondary neutralization of gained pickle liquor sodium hydroxide, pH to 5.5 is adjusted, is added
Thermal response liquid reaction time 1.5h, supplements sodium hydroxide to 85 DEG C during reaction, at the end of reaction, pH terminals are 5.8, instead
Answer liquid to be cooled to 55 DEG C, filtering, be washed to neutrality, obtain pure tellurium dioxide powder, the direct yield of tellurium is 99.76%.
Embodiment 3
A kind of method that tellurium dioxide is extracted in copper ashes from telluride, comprises the following steps：
Step（1）Alkaline pressure of oxygen leaching：By solid-liquid mass ratio 1:7 sodium hydroxide solution and telluride copper ashes by concentration for 150g/L
It is well mixed, it is placed in autoclave, adds appropriate vulcanized sodium, be heated to 140 DEG C, leads to oxygen to 0.7Mpa, keep pressure 4h, treat
Filtered after being cooled to 60 DEG C, the recovery of alkali phase analysis, alkali soaks again；The leaching rate of tellurium is 95.3%.
Step（2）Neutralize heavy tellurium：To step（1）In gained alkali immersion liquid add concentration be 4mol/L sulfuric acid, regulation pH to
5, heating response liquid reaction time 2h, sulfuric acid is supplemented during reaction to 90 DEG C, pH value of solution is maintained 5, at the end of reaction,
PH terminals are 5, and reaction solution is cooled to 60 DEG C, filters while hot, is washed to neutrality, and liquid and neutralization slag after must neutralizing, liquid returns after neutralization
Receive；The yield of tellurium is 99.7%.
Step（3）Salt Ore Leaching：By step（2）Neutralization slag after cleaning is put into 6mol/L hydrochloric acid, controls solid-liquid matter
Amount is than being 1:7, heating response temperature is 85 DEG C, stirs 3h；Chilling temperature obtains pickle liquor and sour slag to filtering after 60 DEG C, acid
Slag continues alkali leaching after telluride copper ashes is included into after stacking and drying, and the leaching rate of hydrochloric acid leaching process is 89.6%；
Step（4）Secondary neutralization：By step（3）The secondary neutralization of gained pickle liquor sodium hydroxide, adjust pH to 6, heating
Reaction solution reaction time 2h, supplements sodium hydroxide to 90 DEG C during reaction, at the end of reaction, pH terminals are 6, and reaction solution is cold
But to 60 DEG C, filtering, neutrality is washed to, obtains pure tellurium dioxide powder, the direct yield of tellurium is 99.6%.
In summary, from telluride copper ashes to pure tellurium dioxide powder, the direct yield of tellurium is more than 86 %, and the rate of recovery can
To reach more than 90%, the purity of tellurium dioxide is more than 99%.
Claims (1)
1. the method for tellurium dioxide is extracted in a kind of copper ashes from telluride, it is characterised in that comprise the following steps：
Step（1）Alkaline pressure of oxygen leaching：By solid-liquid mass ratio 1:5~7 sodium hydroxide solution and telluride copper ashes by concentration for 150g/L
It is well mixed, it is placed in autoclave, adds vulcanized sodium, be heated to 130 ~ 140 DEG C, leads to oxygen to 0.6 ~ 0.7Mpa, keep pressure 3
~ 4h, filtered after being cooled to 50 ~ 60 DEG C, the recovery of alkali phase analysis, alkali soaks again；
Step（2）Neutralize heavy tellurium：To step（1）The sulfuric acid that concentration is 4mol/L is added in gained alkali immersion liquid, adjusts pH to 4~5,
For heating response liquid to 80 ~ 90 DEG C, the reaction time is 1 ~ 2h, and sulfuric acid is supplemented during reaction, pH value of solution is maintained 4.5 ~ 5, reaction
At the end of, pH terminals are 4.5~5, and reaction solution is cooled to 50~60 DEG C, filters while hot, is washed to neutrality, and liquid is with after must neutralizing
And slag, liquid reclaims after neutralization；
Step（3）Salt Ore Leaching：By step（2）Neutralization slag after cleaning is put into 6mol/L hydrochloric acid, controls solid-liquid mass ratio
For 1:6~7, heating response temperature is 75~85 DEG C, stirs 2 ~ 3h；Chilling temperature to filtering after 50~60 DEG C, obtain pickle liquor and
Sour slag, sour slag continue alkali leaching after telluride copper ashes is included into after stacking and drying；
Step（4）Secondary neutralization：By step（3）The secondary neutralization of gained pickle liquor sodium hydroxide, adjusts pH to 5~6, and heating is anti-
Answering liquid, the reaction time is 1 ~ 2h, and sodium hydroxide is supplemented during reaction to 80~90 DEG C, and at the end of reaction, pH terminals are 5.5~6,
Reaction solution is cooled to 50~60 DEG C, filtering, is washed to neutrality, obtains pure tellurium dioxide powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510797529.5A CN105271137B (en) | 2015-11-18 | 2015-11-18 | A kind of method that tellurium dioxide is extracted in the copper ashes from telluride |
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| CN201510797529.5A CN105271137B (en) | 2015-11-18 | 2015-11-18 | A kind of method that tellurium dioxide is extracted in the copper ashes from telluride |
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| CN113337724B (en) * | 2021-06-17 | 2022-08-26 | 安徽工业大学 | Method for synchronously separating and extracting rare-dispersion element tellurium and metal copper from cuprous telluride slag |
| CN113373314B (en) * | 2021-06-17 | 2022-07-29 | 安徽工业大学 | Method for efficiently recycling scattered metal tellurium from cuprous telluride residues |
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| RO86328B1 (en) * | 1983-02-09 | 1985-03-31 | Institutul De Cercetare, Inginerie Tehnologica | Process for preparing tellurium dioxide |
| US8268285B2 (en) * | 2009-06-29 | 2012-09-18 | Pacific Rare Specialty Metals and Chemicals, Inc. | Process for the recovery of tellurium from minerals and/or acidic solutions |
| CN102992280B (en) * | 2011-09-13 | 2015-02-11 | 郴州市金贵银业股份有限公司 | Technology for extracting tellurium dioxide from tellurium-containing smelting slag |
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