CN105217641B - 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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- CN105217641B CN105217641B CN201510677873.0A CN201510677873A CN105217641B CN 105217641 B CN105217641 B CN 105217641B CN 201510677873 A CN201510677873 A CN 201510677873A CN 105217641 B CN105217641 B CN 105217641B
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Abstract
A kind of reduction method of uranium thorium titanium impurity in zircon sand, granularity is that≤200 mesh account for the mass ratio 1 of 96 96.2% zircon sand by zircon sand and 70% sulfuric acid：Feeding leaching is evaporated in device after the sulfuric acid of 0.6 addition 70% is sufficiently mixed, 200 300 degrees Celsius of extraction temperature, extraction time is 12 hours, evaporated temperature is, less than 500 degrees Celsius, to be evaporated the time 30 minutes, and free sulfuric acid is less than 0.5% in the solid zircon sand after being evaporated, solid zircon sand is stirred water logging under 80 100 degrees Celsius, zircon sand solid after water logging is washed under neutrality, 105 degrees Celsius according to 35 times of water of zircon sand quality dries, and produces.Total leaching rate of uranium thorium can be brought up to uranium thorium total amount in 50 70%, zircon sand and be reduced to below 500ppm by the present invention, and titanium oxide is less than 0.2%.So that high radioactivity, the zircon sand of high titanium reach the standard of top grade product.
Description
Technical field
The invention belongs to hydrometallurgy mineral process field, more particularly to uranium thorium ferrotianium aluminium impurity reduction side in zircon sand
Method.
Background technology
At present, granularity<200 mesh account for the processing method bag of uranium thorium ferrotianium aluminium impurity in the zircon sand of 96.2% high uranium thorium titanium
Include Physical and chemical method.Physical is a kind of solid mixed diluting method, and the uranium in original material is not reduced fundamentally
Thorium ferrotianium aluminium impurity.Chemical method is mainly leached using hydrochloric acid, sulfuric acid in normal temperature, and leaching effect is bad, wherein the leaching of uranium
Rate is less than 10%, and the leaching rate of thorium is less than 30%, and titanium-based originally can not be leached.
The content of the invention
It is an object of the invention to provide the reduction side of uranium, thorium, titanium oxide, aluminum oxide, iron oxides impurities in a kind of zircon sand
Method, the impurity effect reduced using this method in zircon sand is good, and uranium thorium total amount is reduced to below 500ppm（Ppm million/
One）, i.e., 0.05%, content of titanium dioxide is reduced to less than 0.2%, and aluminum oxide, the content of iron oxide are reduced to 0.1%, so as to carry
The high purity of zircon sand.
The raw material for using the applicable zircon sand of this method is nature packing density for 2.5-2.55g/cm3, the mesh of granularity≤200
Account for 96-96.2% zircon sand.The method of the present invention, including sulfuric acid leaching and water logging go out.The Ore Leaching stage is carried out by testing
It is preferably as follows：
Specifically, the natural packing density of zircon sand is about 2.5-2.55g/cm in the step of sulfuric acid leaching3, granularity
<200 mesh account for 96.2%, and zircon sand is silicate-type, zircon sand with 70% sulfuric acid reaction it is very faint, it is solid when impurity is with sulfuric acid reaction
The volume of the mixture of body and liquid will not change substantially, and sulfuric acid is easily separated with zircon sand, therefore, in sulfuric acid leaching process
Middle solid-to-liquid ratio is critically important parameter, should ensure to react abundant progress, can not because liquid-solid ratio greatly caused by sulfuric acid prior to solid
Zircon sand is evaporated in device into leaching and is evaporated section, makes to be evaporated the phenomenon that section only evaporates sulfuric acid.Learnt, implemented herein by experiment
The solid-to-liquid ratio of zircon sand and 70% sulfuric acid is 1 in the sulfuric acid leaching section of example:0.6, the extraction temperature during sulfuric acid leaching exists
Between 200-300 degrees Celsius, very slow, 70% sulfuric acid during higher than 300 degrees Celsius that chemical reaction is carried out during less than 200 degrees Celsius
Start a large amount of decomposition, the extraction time of sulfuric acid leaching section is 1-2 hours, during leaching is evaporated, and device is evaporated due to leaching
Axial rotation drives material to be evaporated the asynchronous rotation of device in leaching, and stirring action is played to material.
Show that the solubility of zirconium sulfate in 70% sulfuric acid is minimum by experiment, can so make zirconium dioxide in zircon sand
Composition reduce loss, it is ensured that the reduction of the content of zirconium dioxide is not more than 1% in zircon sand, and impurity titanium, uranium, thorium, iron, aluminium
Solubility it is higher.Boiling point is 338 degrees Celsius to sulfuric acid in mineral acid, in the reaction, can be heated to 300 degrees centigrades.
Therefore, the leaching agent of sulfuric acid leaching section is made using 70% sulfuric acid.
Sulfate after chemical reaction entered with zircon sand leach be evaporated device be evaporated section, this section of temperature of charge is 300-
500 degrees Celsius, at this temperature substantial amounts of sulfuric acid can evaporate or decompose, unnecessary sulfuric acid is evaporated, make in zircon sand
Free sulfuric acid is less than less than 0.5%, and this stage sulfuric acid temperature is not above 550 degrees Celsius, if above 550 degrees Celsius, on the one hand
The sulfate of thorium can form insoluble thorium oxide, so that the leaching rate of thorium is substantially reduced, on the other hand, when temperature is higher than 550
Degree Celsius when can be adsorbed on the surface of zircon sand due to the oxide of iron, the color of zircon sand is become bronzing.
In water logging section, in order to ensure that the sulfate generated in sulfuric acid leaching section is transferred in solution to greatest extent, make solid
Body zircon sand is separated with sulfate impurities.The temperature that make infusion solution in this stage is stirred simultaneously between 80-100 degrees Celsius
Mix 30 minutes.
The solution of water logging section can be recycled for multiple times, and cycle-index is standard less than 40% with the sulfuric acid concentration in solution,
Impurity meeting mass crystallization when sulfuric acid concentration is more than 40% in solution, so that leaching the effect reduction of impurity sulfate.
The main chemical reactions occurred in sulfuric acid leaching section include：
The chemical reaction of sulfuric acid leaching zircon sand uranium：2UO2+O2+ 2H2SO4=2UO2SO4+2H2O；
The chemical reaction of sulfuric acid leaching zircon sand thorium：ThO2+2H2SO4= Th(SO4)2+2H2O ；
The reaction of sulfuric acid and zirconium silicate is very faint：ZrSiO4+2H2SO4= Zr(SO4)2+2H2O+ SiO2；
The chemical reaction of sulfuric acid and di-iron trioxide：3H2SO4 +Fe2O3= Fe2(SO4)3+3H2O ；
The chemical reaction of sulfuric acid and alundum (Al2O3)：3H2SO4 + Al2O3= Al2(SO4)3+3H2O ；
The chemical reaction of sulfuric acid and titanium dioxide：2H2SO4 + TiO2= Ti(SO4)2+2H2O 。
Above-mentioned leaching drier carries out axial rotation with 45 revolutions per seconds of rotating speed, leaches angle≤3 of drier and horizontal plane
O, the inlet temperature for leaching drier is >=200 DEG C.
The preferred method of the present invention is in summary：
A kind of reduction method of uranium thorium titanium impurity in zircon sand, it is characterised in that：
It is derived from right packing density 2.5-2.55g/cm3, granularity is that≤200 mesh account for 96-96.2% zircon sand raw material by zirconium English
The mass ratio 1 of sand and 70% sulfuric acid：Feeding leaching, which is evaporated in device, after the sulfuric acid of 0.6 addition 70% is sufficiently mixed is leached
It is evaporated, 200-300 degrees Celsius of extraction temperature, extraction time is 1-2 hours, evaporated temperature is, less than 500 degrees Celsius, to be evaporated the time
30 minutes, free sulfuric acid was less than 0.5% in the solid zircon sand after being evaporated, and solid zircon sand is stirred under 80-100 degrees Celsius
Water logging is mixed, the zircon sand solid after water logging is washed under neutrality, 105 degrees Celsius according to 3-5 times of water of zircon sand quality to be dried
It is dry, produce.
Above-mentioned leaching drier carries out axial rotation with 45 revolutions per seconds of rotating speed, leaches the angle≤3o dried with horizontal plane,
Leach inlet temperature >=200 DEG C of drier.
Present invention process is simple, and total leaching rate of uranium thorium can be brought up to uranium thorium total amount in 50-70%, zircon sand to be reduced
To below 500ppm, titanium oxide is reduced to less than 0.1% less than 0.2%, iron oxide and aluminum oxide.So that high radioactivity, Gao Tai
Zircon sand reach the standards of top grade product.
Brief description of the drawings
Fig. 1 is uranium thorium ferrotianium aluminium impurity reduction method flow diagram in zircon sand provided in an embodiment of the present invention.
Embodiment
Embodiment one
Uranium thorium ferrotianium aluminium impurity reduces method in a kind of zircon sand, comprises the following steps：
By granularity be 80-140 mesh account for 0.44%, 140-160 mesh account for 0.69%, 160-200 mesh account for 2.57%≤200 mesh account for
96.2% zircon sand and 70% sulfuric acid are according to mass ratio 1:Feeding leaching, which is evaporated in device, after 0.6 ratio is mixed is soaked
Go out to be evaporated, 300 degrees Celsius of extraction temperature, extraction time 2 hours, evaporated temperature is, less than 500 degrees Celsius, to be evaporated 30 points of time
Free sulfuric acid is less than 0.5% in clock, the solid zircon sand after being evaporated, and solid zircon sand is stirred water logging under 100 degrees Celsius,
Zircon sand solid after water logging is washed under neutrality, 105 degrees Celsius according to 5 times of water of zircon sand quality dries, and produces.
Embodiment two
A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand, be≤200 mesh are accounted for 96.2% zircon sand and 70%
Sulfuric acid according to mass ratio 1:Feeding leaching is evaporated progress leaching in device and is evaporated after 0.6 ratio is mixed, extraction temperature 280
Degree Celsius, extraction time 1.8 hours, evaporated temperature is, less than 500 degrees Celsius, to be evaporated the time 30 minutes, the solid zirconium after being evaporated
Free sulfuric acid is less than 0.5% in sand, and solid zircon sand is stirred water logging at 80 degrees celsius, the zircon sand solid after water logging
3 times of the water according to zircon sand quality is washed under neutrality, 105 degrees Celsius and dried, and produces.
Embodiment three
A kind of reduction method of uranium thorium ferrotianium aluminium impurity in zircon sand, be≤200 mesh are accounted for 96.2% zircon sand and 70%
Sulfuric acid according to mass ratio 1:Feeding leaching is evaporated progress leaching in device and is evaporated after 0.6 ratio is mixed, extraction temperature 260
DEG C, extraction time 1.5 hours, evaporated temperature is, less than 500 degrees Celsius, to be evaporated the time 30 minutes, the solid zircon sand after being evaporated
Middle free sulfuric acid is less than 0.5%, and solid zircon sand is stirred water logging at 85 DEG C, and the zircon sand solid after water logging is according to zirconium English
4.5 times of water of chiltern amount is washed under neutrality, 105 degrees Celsius and dried, and produces.
Claims (2)
1. a kind of reduction method of uranium thorium titanium impurity in zircon sand, it is characterised in that：
It is derived from right packing density 2.5-2.55g/cm3, granularity be≤200 mesh account for 96-96.2% zircon sand raw material by zircon sand with
The mass ratio 1 of 70% sulfuric acid：Feeding leaching is evaporated progress leaching steaming in device after the sulfuric acid of 0.6 addition 70% is sufficiently mixed
Dry, 200-300 degrees Celsius of extraction temperature, extraction time is 1-2 hours, and evaporated temperature is, less than 500 degrees Celsius, to be evaporated the time 30
Minute, free sulfuric acid is less than 0.5% in the solid zircon sand after being evaporated, and solid zircon sand is stirred under 80-100 degrees Celsius
Water logging, the zircon sand solid after water logging is washed under neutrality, 105 degrees Celsius according to 3-5 times of water of zircon sand quality dries,
Produce.
2. the reduction method of uranium thorium titanium impurity in a kind of zircon sand according to claim 1, it is characterised in that：Leach drying
Device carries out axial rotation with 45 revolutions per seconds of rotating speed, leaches angle≤3o of drier and horizontal plane, leaches the import temperature of drier
>=200 DEG C of degree.
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| EP3256424A4 (en) * | 2015-02-09 | 2018-08-01 | Iluka Resources Limited | Process for improving the grade and optical quality of zircons |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| AU2021221762B2 (en) * | 2021-08-25 | 2024-01-18 | Australian Nuclear Science And Technology Organisation | Mineral sand particulate processing |
| AU2021221764B2 (en) * | 2021-08-25 | 2024-02-08 | Australian Nuclear Science And Technology Organisation | Processing of mineral sand particulates |
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| CN103466697A (en) * | 2013-09-10 | 2013-12-25 | 圣泉（福建）制釉有限公司 | Preparation method and application of active zirconium dioxide |
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| CN101407597A (en) * | 2007-10-12 | 2009-04-15 | 上海化工研究院 | Halogen-free flame-retardant photo-curing epoxy resin composition |
| CN103253700A (en) * | 2012-02-15 | 2013-08-21 | 淄博市周村磊宝耐火材料有限公司 | Method for purification of zircon sand to prepare high purity zirconia |
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