CN105217641A - A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand - Google Patents
A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand Download PDFInfo
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- CN105217641A CN105217641A CN201510677873.0A CN201510677873A CN105217641A CN 105217641 A CN105217641 A CN 105217641A CN 201510677873 A CN201510677873 A CN 201510677873A CN 105217641 A CN105217641 A CN 105217641A
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- zircon sand
- evaporate
- dryness
- sulfuric acid
- solid
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000004576 sand Substances 0.000 title claims abstract description 69
- 229910052845 zircon Inorganic materials 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000012535 impurity Substances 0.000 title claims abstract description 20
- GFRMDONOCHESDE-UHFFFAOYSA-N [Th].[U] Chemical compound [Th].[U] GFRMDONOCHESDE-UHFFFAOYSA-N 0.000 title abstract description 14
- 239000004411 aluminium Substances 0.000 title description 10
- 229910052782 aluminium Inorganic materials 0.000 title description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000002386 leaching Methods 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- -1 uranium thorium titanium Chemical compound 0.000 claims abstract description 5
- 238000012856 packing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000010936 titanium Substances 0.000 abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 12
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052776 Thorium Inorganic materials 0.000 description 6
- 229910052770 Uranium Inorganic materials 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000001018 Hibiscus sabdariffa Nutrition 0.000 description 1
- 235000005291 Rumex acetosa Nutrition 0.000 description 1
- 240000007001 Rumex acetosella Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910006501 ZrSiO Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000003978 infusion fluid Substances 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000003513 sheep sorrel Nutrition 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of reduction method of uranium thorium titanium impurity in zircon sand, sending into after the granularity sulfuric acid that to be≤200 orders zircon sand that accounts for 96-96.2% add 70% by zircon sand and the mass ratio 1:0.6 of the sulfuric acid of 70% carries out fully mixing leaches in evaporate to dryness device, extraction temperature 200-300 degree Celsius, extraction time is 1-2 hour, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging under 80-100 degree Celsius, zircon sand solid after water logging is washed to neutrality according to the 3-5 water yield doubly of zircon sand quality, dry under 105 degrees Celsius, obtain.Total leaching yield of uranium thorium can be brought up to 50-70% by the present invention, and in zircon sand, uranium thorium total amount is reduced to below 500ppm, and titanium oxide is lower than 0.2%.Thus make high radioactivity, standard that the zircon sand of high titanium reaches top grade product.
Description
Technical field
The invention belongs to hydrometallurgy mineral processing field, particularly relate to uranium thorium ferrotianium aluminium impurity reduction method in zircon sand.
Background technology
At present, the treatment process that granularity <200 order accounts for uranium thorium ferrotianium aluminium impurity in the zircon sand of the high uranium thorium titanium of 96.2% comprises Physical and chemical method.Physical is a kind of solids mixing dilution process, does not fundamentally reduce the uranium thorium ferrotianium aluminium impurity in original material.Chemical method mainly adopts hydrochloric acid, sulfuric acid leaches at normal temperature, and leaching effect is bad, and wherein the leaching yield of uranium is less than 10%, and the leaching yield of thorium is less than 30%, and titanium can not leach substantially.
Summary of the invention
The object of this invention is to provide a kind of reduction method of uranium, thorium, titanium oxide, aluminum oxide, iron oxides impurities in zircon sand, the impurity adopting the method to reduce in zircon sand is effective, uranium thorium total amount is reduced to below 500ppm (ppm 1,000,000/), namely 0.05%, content of titanium dioxide is reduced to less than 0.2%, the content of aluminum oxide, ferric oxide is reduced to 0.1%, thus improves the purity of zircon sand.
The raw material of the zircon sand adopting present method to be suitable for is nature packing density is 2.5-2.55g/cm
3, granularity≤200 order accounts for the zircon sand of 96-96.2%.Method of the present invention, comprises sulfuric acid leaching and water logging goes out.The Ore Leaching stage is preferably as follows by test:
Particularly, in this step of sulfuric acid leaching, the natural packing density of zircon sand is about 2.5-2.55g/cm
2granularity <200 order accounts for 96.2%, zircon sand is silicate-type, zircon sand and 70% sulfuric acid reaction very faint, when impurity and sulfuric acid reaction, the volume of the mixture of solid and liquid can not change substantially, sulfuric acid and zircon sand are easy to be separated, therefore, in sulfuric acid leaching process, solid-to-liquid ratio is very important parameter, should ensure that sufficient reacting carries out, sulfuric acid can not be caused greatly prior to solid zircon sand to enter the evaporate to dryness section leached in evaporate to dryness device because of liquid-solid ratio, make evaporate to dryness section only evaporate the phenomenon of sulfuric acid.Learn by experiment, in the sulfuric acid leaching section of this embodiment zircon sand and 70% the solid-to-liquid ratio of sulfuric acid be 1:0.6, extraction temperature in sulfuric acid leaching process is between 200-300 degree Celsius, what when being less than 200 degrees Celsius, chemical reaction carried out is very slow, higher than when 300 degrees Celsius 70% sulfuric acid start a large amount of decomposition, the extraction time of sulfuric acid leaching section is 1-2 hour, in leaching evaporate to dryness process, because the axial rotation leaching evaporate to dryness device drives material in the asynchronous rotation of leaching evaporate to dryness device, stirring action is played to material.
Show that the solubleness of zirconium sulfate in the sulfuric acid of 70% is minimum by experiment, the composition of zirconium dioxide in zircon sand can be made like this to reduce the loss, ensure that the minimizing of the content of zirconium dioxide in zircon sand is not more than 1%, and the solubleness of impurity titanium, uranium, thorium, iron, aluminium is higher.Sulfuric acid in mineral acid boiling point is 338 degrees Celsius, in the reaction, can be heated to 300 degrees centigrade.Therefore, the sulfuric acid of 70% is used to make the leaching agent of sulfuric acid leaching section.
Vitriol after chemical reaction enters into the evaporate to dryness section leaching evaporate to dryness device with zircon sand, this section of temperature of charge is 300-500 degree Celsius, sulfuric acid a large amount of at this temperature can evaporate or decompose, unnecessary sulfuric acid is evaporated away, the free sulfuric acid in zircon sand is made to be less than less than 0.5%, this stage sulfuric acid temperature can not higher than 550 degrees Celsius, if higher than 550 degrees Celsius, the vitriol of thorium can form insoluble Thorotrast on the one hand, thus the leaching yield of thorium is reduced greatly, on the other hand, when temperature can be adsorbed on the surface of zircon sand higher than the oxide compound due to iron when 550 degrees Celsius, the color of zircon sand is made to become sorrel.
In water logging section, in order to ensure that the vitriol generated in sulfuric acid leaching section is transferred in solution to greatest extent, solid zircon sand is separated with sulfate impurities.To make the temperature of infusion solution between 80-100 degree Celsius in this stage, stir 30 minutes simultaneously.
The solution of water logging section can repeatedly recycle, and cycle index is less than 40% for standard with the sulfuric acid concentration in solution, and impurity when sulfuric acid concentration is greater than 40% in solution can mass crystallization, thus the effect of leaching sulfur impurity hydrochlorate is reduced.
The main chemical reactions occurred in sulfuric acid leaching section comprises:
The chemical reaction of sulfuric acid leaching zircon sand uranium: 2UO
2+ O
2+ 2H
2sO
4=2UO
2sO
4+ 2H
2o;
The chemical reaction of sulfuric acid leaching zircon sand thorium: ThO
2+ 2H
2sO
4=Th (SO
4)
2+ 2H
2o;
The reaction of sulfuric acid and zirconium silicate is very faint: ZrSiO
4+ 2H
2sO
4=Zr (SO
4)
2+ 2H
2o+SiO
2;
The chemical reaction of sulfuric acid and ferric oxide: 3H
2sO
4+ Fe
2o
3=Fe
2(SO
4)
3+ 3H
2o;
The chemical reaction of sulfuric acid and aluminium sesquioxide: 3H
2sO
4+ Al
2o
3=Al
2(SO
4)
3+ 3H
2o;
The chemical reaction of sulfuric acid and titanium dioxide: 2H
2sO
4+ TiO
2=Ti (SO
4)
2+ 2H
2o.
Above-mentioned leaching moisture eliminator carries out axial rotation with the rotating speed of 45 revolutions per seconds, leaches the angle≤3o of moisture eliminator and horizontal plane, and the inlet temperature leaching moisture eliminator is >=200 DEG C.
The preferred method of the present invention is in sum:
A reduction method for uranium thorium titanium impurity in zircon sand, is characterized in that:
Take from right packing density 2.5-2.55g/cm, send into leach in evaporate to dryness device after the granularity sulfuric acid that to be≤200 orders zircon sand raw material that accounts for 96-96.2% add 70% by zircon sand and the mass ratio 1:0.6 of the sulfuric acid of 70% carries out fully mixing and carry out leaching evaporate to dryness, extraction temperature 200-300 degree Celsius, extraction time is 1-2 hour, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging under 80-100 degree Celsius, zircon sand solid after water logging is washed to neutrality according to the 3-5 water yield doubly of zircon sand quality, dry under 105 degrees Celsius, obtain.
Above-mentioned leaching moisture eliminator carries out axial rotation with the rotating speed of 45 revolutions per seconds, leaches angle≤3o that is dry and horizontal plane, leaches inlet temperature >=200 DEG C of moisture eliminator.
Present invention process is simple, and total leaching yield of uranium thorium can be brought up to 50-70%, in zircon sand, uranium thorium total amount is reduced to below 500ppm, titanium oxide lower than 0.2%, ferric oxide and aluminum oxide be reduced to less than 0.1%.Thus make high radioactivity, standard that the zircon sand of high titanium reaches top grade product.
Accompanying drawing explanation
Fig. 1 is that in the zircon sand that provides of the embodiment of the present invention, uranium thorium ferrotianium aluminium impurity reduces method flow diagram.
Embodiment
Embodiment one
A kind of uranium thorium ferrotianium aluminium impurity reduction method in zircon sand, comprises the steps:
Be that 80-140 order accounts for 0.44% by granularity, 140-160 order accounts for 0.69%, 160-200 order account for 2.57%≤200 orders account for the zircon sand of 96.2% and the sulfuric acid of 70% according to the ratio of mass ratio 1:0.6 carry out mixing rear send into leach in evaporate to dryness device carry out leaching evaporate to dryness, extraction temperature 300 degrees Celsius, extraction time 2 hours, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging under 100 degrees Celsius, zircon sand solid after water logging is washed to neutrality according to the water yield of 5 times of zircon sand quality, dry under 105 degrees Celsius, obtain.
Embodiment two
A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand, be≤200 orders are accounted for the zircon sand of 96.2% and the sulfuric acid of 70% according to the ratio of mass ratio 1:0.6 carry out mixing rear send into leach in evaporate to dryness device carry out leaching evaporate to dryness, extraction temperature 280 degrees Celsius, extraction time 1.8 hours, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging at 80 degrees celsius, zircon sand solid after water logging is washed to neutrality according to the water yield of 3 times of zircon sand quality, dry under 105 degrees Celsius, obtain.
Embodiment three
A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand, be≤200 orders are accounted for the zircon sand of 96.2% and the sulfuric acid of 70% according to the ratio of mass ratio 1:0.6 carry out mixing rear send into leach in evaporate to dryness device carry out leaching evaporate to dryness, extraction temperature 260 DEG C, extraction time 1.5 hours, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging at 85 DEG C, zircon sand solid after water logging is washed to neutrality according to the water yield of 4.5 times of zircon sand quality, dry under 105 degrees Celsius, obtain.
Claims (2)
1. the reduction method of uranium thorium titanium impurity in zircon sand, is characterized in that:
Take from right packing density 2.5-2.55g/cm, send into leach in evaporate to dryness device after the granularity sulfuric acid that to be≤200 orders zircon sand raw material that accounts for 96-96.2% add 70% by zircon sand and the mass ratio 1:0.6 of the sulfuric acid of 70% carries out fully mixing and carry out leaching evaporate to dryness, extraction temperature 200-300 degree Celsius, extraction time is 1-2 hour, evaporate to dryness temperature is for being less than 500 degrees Celsius, 30 minutes evaporate to dryness time, solid zircon sand Free Sulfuric Acid after evaporate to dryness is less than 0.5%, solid zircon sand carries out stirring water logging under 80-100 degree Celsius, zircon sand solid after water logging is washed to neutrality according to the 3-5 water yield doubly of zircon sand quality, dry under 105 degrees Celsius, obtain.
2. the reduction method of uranium thorium titanium impurity in a kind of zircon sand according to claim 1, it is characterized in that: leach moisture eliminator and carry out axial rotation with the rotating speed of 45 revolutions per seconds, leach the angle≤3o of moisture eliminator and horizontal plane, leach inlet temperature >=200 DEG C of moisture eliminator.
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| Publication Number | Publication Date |
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| CN105217641B CN105217641B (en) | 2017-10-27 |
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Cited By (7)
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|---|---|---|---|---|
| CN105502423A (en) * | 2016-01-28 | 2016-04-20 | 郭志斌 | Method for producing high-grade zircon sand |
| CN112694326A (en) * | 2020-12-30 | 2021-04-23 | 泉州市利芝新材料科技有限公司 | Zircon sand iron removal process |
| CN112723366A (en) * | 2020-12-30 | 2021-04-30 | 泉州市利芝新材料科技有限公司 | Process for removing iron and titanium from zircon sand |
| US11066726B2 (en) | 2015-02-09 | 2021-07-20 | Iluka Resources Limited | Process for improving the grade and optical quality of zircons |
| AU2021266303A1 (en) * | 2021-08-25 | 2023-03-16 | Australian Nuclear Science And Technology Organisation | Processing of mineral sand particulates |
| AU2021221762B2 (en) * | 2021-08-25 | 2024-01-18 | Australian Nuclear Science And Technology Organisation | Mineral sand particulate processing |
| WO2024173995A1 (en) * | 2023-02-24 | 2024-08-29 | Iluka Resources Limited | Process and apparatus |
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| US11066726B2 (en) | 2015-02-09 | 2021-07-20 | Iluka Resources Limited | Process for improving the grade and optical quality of zircons |
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| WO2024173995A1 (en) * | 2023-02-24 | 2024-08-29 | Iluka Resources Limited | Process and apparatus |
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| Publication number | Publication date |
|---|---|
| CN105217641B (en) | 2017-10-27 |
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