CN115710648B - Method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore - Google Patents
Method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore Download PDFInfo
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- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 title claims abstract description 49
- 229910052776 Thorium Inorganic materials 0.000 title claims abstract description 49
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 43
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 23
- VMVMGFKIKJPPNF-UHFFFAOYSA-N [Ce].[Ti].[Si] Chemical compound [Ce].[Ti].[Si] VMVMGFKIKJPPNF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000012141 concentrate Substances 0.000 claims abstract description 64
- 238000002386 leaching Methods 0.000 claims abstract description 44
- 238000007885 magnetic separation Methods 0.000 claims abstract description 26
- 239000002893 slag Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims description 10
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 9
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000010517 secondary reaction Methods 0.000 claims description 8
- 239000003929 acidic solution Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000004537 pulping Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910000175 cerite Inorganic materials 0.000 claims 1
- 238000011010 flushing procedure Methods 0.000 claims 1
- 238000005065 mining Methods 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 241000777300 Congiopodidae Species 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000020477 pH reduction Effects 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000006148 magnetic separator Substances 0.000 description 2
- 229910052674 natrolite Inorganic materials 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910001727 uranium mineral Inorganic materials 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 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 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- GFRMDONOCHESDE-UHFFFAOYSA-N [Th].[U] Chemical compound [Th].[U] GFRMDONOCHESDE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 229910052612 amphibole Inorganic materials 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052663 cancrinite Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000010423 industrial mineral Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 229910052664 nepheline Inorganic materials 0.000 description 1
- 239000010434 nepheline Substances 0.000 description 1
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 239000010435 syenite Substances 0.000 description 1
- 229910052847 thorite Inorganic materials 0.000 description 1
- XSSPKPCFRBQLBU-UHFFFAOYSA-N thorium(iv) orthosilicate Chemical compound [Th+4].[O-][Si]([O-])([O-])[O-] XSSPKPCFRBQLBU-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- -1 transuranite Inorganic materials 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the field of ore mining and smelting, in particular to a method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore. The method comprises the following steps: grinding the green layer silicon-cerium titanium ore to obtain coarse ore with the thickness of-1-0 mm; wherein, coarse ore with the diameter of-0.074-0 mm is used as ore slurry to enter bulk concentrate; feeding the coarse ore with the diameter of-1+0.074 mm into the next step of two-stage magnetic separation; carrying out first-stage magnetic separation on coarse ore with the magnetic field strength of 10000-11000 Oerst and the coarse ore with the magnetic field strength of-1+0.074 mm, and taking the passed ore as concentrate to enter bulk concentrate; carrying out second-stage magnetic separation on the ores which do not pass through by using a magnetic field with the intensity of 12000-13000 Oerst, and enabling the passing part to enter bulk concentrates; countercurrent leaching is carried out on the bulk concentrate, and uranium and thorium in the bulk concentrate are extracted; adding alkali into the leached slag for treatment, then reacting with dilute sulfuric acid, and extracting thorium. The invention leaches uranium and comprehensively recovers thorium, and has high leaching rate of uranium and thorium.
Description
Technical Field
The invention relates to the field of ore mining and smelting, in particular to a method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore.
Background
The Liaoning Fengcheng racehorse alkaline uranium deposit is a comprehensive deposit of uranium, thorium and rare earth elements with large scale, is unique in China and is rare in the world. The deposit has attracted considerable attention from the uranium ore geology and mining community since its discovery in the 70 s of the last century. Some leaching tests are performed at the moment, but the uranium leaching rate and the comprehensive utilization rate of other ore species are difficult to solve due to technical reasons.
The racehorse uranium deposit is produced in alkaline rock. The main uranium ore type is the green layer silcerite mineralization produced in grass green neon syenite. It constitutes the main body of large-scale comprehensive ore deposit of racehorse uranium, thorium, rare earth and niobium. The industrial minerals are green-layer silicon cerium titanium and changed minerals with different degrees. The uranium content is changed between 0.05% and 0.1%, the thorium content is between 0.15% and 0.4%, and the cerium rare earth element and the niobium content meet the industrial requirements.
Green layer silicon-cerium-titanium ore is a rare type of uranium mineral in the world. Because most of minerals belong to aluminosilicate or iron silicate types and contain rare earth, thorium, niobium tantalum and other components, uranium minerals are difficult to leach, and when the conventional acid method is adopted for leaching, the acid consumption is high, the leaching rate is low, and solid-liquid separation of ore pulp after leaching is difficult.
Disclosure of Invention
The invention aims to solve the technical problems that: the method for extracting uranium and thorium from the green-layer silicon-cerium-titanium ore is provided, the uranium is leached, the thorium is comprehensively recovered, and the leaching rate of the uranium and the thorium is high.
The invention provides a method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore, which comprises the following steps:
step S1: grinding the green layer silicon-cerium titanium ore to obtain coarse ore with the thickness of-1-0 mm; wherein, coarse ore with the diameter of-0.074-0 mm is used as ore slurry to enter bulk concentrate;
feeding the coarse ore with the diameter of-1+0.074 mm into the next step of two-stage magnetic separation;
step S2: carrying out first-stage magnetic separation on coarse ore with the magnetic field strength of 10000-11000 Oerst and the coarse ore with the magnetic field strength of-1+0.074 mm, and taking the passed ore as concentrate to enter bulk concentrate;
carrying out second-stage magnetic separation on the non-passing ores by using a magnetic field with the intensity of 12000-13000 Oerst, wherein the passing part enters bulk concentrate, and the non-passing ores are tailings;
step S3: countercurrent leaching is carried out on the bulk concentrate, and uranium and thorium in the bulk concentrate are extracted;
step S4: and (3) adding alkali into the leaching slag in the step (S3) for treatment, and then reacting with dilute sulfuric acid to extract thorium.
Preferably, in the step S2: and carrying out first-stage magnetic separation on the coarse ore with the magnetic field strength of 10500-10700 Oersted to obtain coarse ore with the magnetic field strength of-1+0.074 mm.
Preferably, the step S3 specifically includes:
adding sulfuric acid, calcium fluoride and manganese dioxide into the bulk concentrate, stirring, fully reacting, adding water, sulfuric acid and manganese dioxide for secondary reaction, and filtering after the secondary reaction is finished; collecting filtrate;
adding an acidic solution into the obtained filter residues, stirring, and pulping for 2-5 times;
washing leaching residues.
Preferably, the grain size of the bulk concentrate is-0.417 mm to-0.074 mm.
Preferably, based on the mass of bulk concentrate, 22% sulfuric acid, 3% calcium fluoride and 1% manganese dioxide are added into 100g of bulk concentrate with the particle size of-0.208 mm, and the liquid-solid ratio of sulfuric acid to ore is 1.2:1, stirring and reacting for 2 hours at 120 ℃.
Preferably, 200ml of water, 3% sulfuric acid, 1% manganese dioxide are added and the secondary reaction is carried out at 80℃for 2 hours.
Preferably, the step S4 specifically includes:
100g of ammonium hydroxide with the mass concentration of 25% is added into the leaching residue in the step S3, and the mixture is stirred and filtered after full reaction; collecting filtrate;
acidifying the filter residue with 0.5-1% sulfuric acid, washing with acidified water with pH value of 1.5 for 3-5 times, stirring for 15 min during each washing, and filtering; collecting filter residues;
the filter residue is rinsed with water, and the tailings are reserved.
Preferably, in the step S4,
100g of leaching slag in the step S3 with the solid-liquid ratio of 1.2:1 is added with 0.8-1.8 ml of ammonium hydroxide with the concentration of 25%, stirred, fully reacted and filtered; the filtrate was collected.
Preferably, in the step S4,
100g of leaching slag in the step S3 with the solid-liquid ratio of 1.2:1 is added with 1ml of ammonium hydroxide with the concentration of 25 percent, stirred for 0.25 to 1 hour, fully reacted and filtered; the filtrate was collected.
Preferably, in the step S4,
acidifying the filter residue with 0.5% sulfuric acid, washing with acidified water with pH value of 1.5 for 3-5 times, stirring for 15 min during each washing, and filtering; and (5) collecting filter residues.
Compared with the prior art, the method for extracting uranium and thorium from the green-layer silicon-cerium-titanium ore has the advantages that firstly, dry magnetic separation is carried out to obtain bulk concentrate, and countercurrent leaching is carried out on the bulk concentrate to leach uranium and thorium; and converting the countercurrent leaching slag by adopting a conversion treatment to convert sulfuric acid double salt of thorium into hydroxide, and then carrying out dilute sulfuric acid treatment to further extract thorium. According to the invention, the comprehensive recovery of the thorium is carried out while the uranium is leached, and the uranium leaching rate is high.
Drawings
Fig. 1 shows a flow chart of dry magnetic separation.
Detailed Description
For a further understanding of the present invention, embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the invention.
The embodiment of the invention discloses a method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore, which comprises the following steps:
step S1: grinding the green layer silicon-cerium titanium ore to obtain coarse ore with the thickness of-1-0 mm; wherein, coarse ore with the diameter of-0.074-0 mm is used as ore slurry to enter bulk concentrate;
feeding the coarse ore with the diameter of-1+0.074 mm into the next step of two-stage magnetic separation;
step S2: carrying out first-stage magnetic separation on coarse ore with the magnetic field strength of 10000-11000 Oerst and the coarse ore with the magnetic field strength of-1+0.074 mm, and taking the passed ore as concentrate to enter bulk concentrate;
carrying out second-stage magnetic separation on the non-passing ores by using a magnetic field with the intensity of 12000-13000 Oerst, wherein the passing part enters bulk concentrate, and the non-passing ores are tailings;
step S3: countercurrent leaching is carried out on the bulk concentrate, and uranium and thorium in the bulk concentrate are extracted;
step S4: and (3) adding alkali into the leaching slag in the step (S3) for treatment, and then reacting with dilute sulfuric acid to extract thorium.
According to the invention, the ore is first subjected to dry magnetic separation. Specifically:
step S1: grinding the green layer silicon-cerium titanium ore to obtain coarse ore with the thickness of-1-0 mm; wherein, coarse ore with the diameter of-0.074-0 mm is used as ore slurry to enter bulk concentrate;
feeding the coarse ore with the diameter of-1+0.074 mm into the next step of two-stage magnetic separation;
step S2: performing primary magnetic separation on coarse ore with the magnetic field strength of 10000-11000 Oersted, preferably 10500-10700 Oersted, more preferably 10600 Oersted, wherein the coarse ore with the magnetic field strength of-1+0.074 mm is used as concentrate, and the passing ore enters bulk concentrate;
and carrying out second-stage magnetic separation on the non-passing ore by using a magnetic field with the strength of 12000-13000 Oerst, preferably 12000 Oerst, wherein the passing part enters bulk concentrate, and the non-passing ore is tailings. The non-passing tailings are discarded.
After obtaining bulk concentrates, the bulk concentrates are leached in countercurrent, in particular:
step S3: and (3) countercurrent leaching is carried out on the bulk concentrate, and uranium and thorium in the bulk concentrate are extracted.
The step S3 specifically includes:
adding sulfuric acid, calcium fluoride and manganese dioxide into the bulk concentrate, stirring, fully reacting, adding water, sulfuric acid and manganese dioxide for secondary reaction, and filtering after the secondary reaction is finished; collecting filtrate;
adding an acidic solution into the obtained filter residues, stirring, and pulping for 2-5 times;
washing leaching residues.
The particle size of the bulk concentrate is preferably-0.417 mm to-0.074 mm, and more preferably-0.208 mm.
Preferably, based on the mass of bulk concentrate, 22% sulfuric acid, 3% calcium fluoride and 1% manganese dioxide are added into 100g of bulk concentrate with the particle size of-0.208 mm, and the liquid-solid ratio of sulfuric acid to ore is 1.2:1, stirring and reacting for 2 hours at 120 ℃.
22% sulfuric acid refers to the addition amount of 22% of the mass of bulk concentrate as sulfuric acid; 3% of calcium fluoride and 1% of manganese dioxide are similar in meaning, and all refer to the addition amount taking bulk concentrate as a standard.
Then, 200ml of water was added, 3% sulfuric acid and 1% manganese dioxide were added, and the reaction was carried out at 80℃for 2 hours.
3% sulfuric acid and 1% manganese dioxide refer to the addition amount taking bulk concentrate as a standard.
Adding an acidic solution into the obtained filter residue, stirring for 15 minutes, and pulping for 2-5 times, preferably 3 times;
washing the leaching residue with tap water.
The obtained leaching slag is further subjected to alkali conversion to extract thorium. The method specifically comprises the following steps:
step S4: and (3) adding alkali into the leaching slag in the step (S3) for treatment, and then reacting with dilute sulfuric acid to extract thorium.
The mass percentage concentration of the dilute sulfuric acid is less than 70%.
Preferably, the step S4 specifically includes:
100g of ammonium hydroxide with the mass concentration of 25% and the solid-liquid ratio of 1.2:1 is added into the leaching slag in the step S3, and the mixture is stirred for 0.25 to 1 hour, and filtered after full reaction; collecting filtrate;
acidifying the filter residue with 0.5-1% sulfuric acid, washing with acidified water with pH value of 1.5 for 3-5 times, stirring for 15 min during each washing, and filtering; collecting filter residues;
the filter residue is rinsed with water, and the tailings are reserved.
The 0.5-1% sulfuric acid refers to the sulfuric acid added with the mass of filter residues as the standard, and the sulfuric acid is 0.5-1%.
More preferably, adding 4ml of ammonium hydroxide with mass concentration of 25% into 100g of leaching slag in the step S3 with solid-to-liquid ratio of 1.2:1, stirring for 0.25 hour, and filtering after full reaction; collecting filtrate;
acidifying the filter residue with 0.5% sulfuric acid, washing with acidified water with pH of 1.5 for 3 times, stirring for 15 min each time, and filtering; collecting filter residues;
the filter residue is rinsed with water, and the tailings are reserved.
For further understanding of the present invention, the following examples are provided to illustrate the extraction of uranium and thorium from green-layer bastnaesite in detail, and the scope of the present invention is not limited by the following examples.
Example 1
Mineral separation (I)
The ore has a plurality of ore types. The main minerals include feldspar (about 40%), nepheline (about 2 0%), neon stone, spodumene (about 25%) and green-layer siliconite. The secondary minerals include collodion-green layer silicon-cerium titanium ore, foreign stone, amphibole, needle natrolite, cancrinite, uranium thorite, natrolite, etc.; there are also small amounts of titanium columbium-calcium cerium ore, sodium zircon, fluorite, transuranite, and metal sulphide minerals. The main industrially useful mineral is green-layer silicon-cerium-titanium ore and its alteration products.
100kg of green-layer silicon-cerium titanium ore is taken from the racehorse deposit, and is ground and reduced.
1. Dry magnetic separation
Step 1: grinding: the uranium grade of the ore is 0.055 percent and the thorium grade is 0.171 percent. Grinding the raw ore by a rod mill to 1-0 mm.
Step 2: and (3) screening: -a fraction of 0.074-0 mm is fed as slurry into the bulk concentrate. The concentrate yield is 71.17%, the uranium grade is 0.073%, and the thorium grade is 0.226%.
Step 3: -1+0.074mm section, two-stage magnetic separation.
(1) First-stage magnetic separation: the magnetic field strength was 10600 oersted (138T-C M single roll magnetic separator) and passed through a portion of the ore as concentrate into bulk concentrate. The non-passed portion of the ore was subjected to a second stage magnetic separation as shown in figure 1.
(2) And the second stage of magnetic separation, namely a single-roller magnetic separator with the magnetic field strength of 12000 Oerst (138T-C.comprise M). Through part of the ore as concentrate into bulk concentrate. Part of the ores which do not pass through are discarded as tailings (the uranium grade of the tailings is 0.0098 percent and the thorium grade is 0.036 percent).
2. Magnetic concentrate particle size selection
From the magnetic concentrate particle size test, the optimum particle size was selected to be-0.208 mm as shown in table 1.
Table 1 particle size test of magnetic concentrate
Counter current leaching of uranium thorium in bulk concentrate
1. Leaching uranium and thorium mixed concentrate
The test conditions and method steps are as follows:
step 1:100g of bulk concentrate with the thickness of-0.208 mm is added with 22 percent of sulfuric acid, 30 percent of calcium fluoride and 10 percent of manganese dioxide, and the liquid-solid ratio of sulfuric acid to ore is 1.2:1, stirring.
Step 2: drying at 120deg.C for 2 hr, adding 200ml water, and adding 30% sulfuric acid and 10% manganese dioxide.
Step 3: leaching with stirring in a water bath at 80deg.C for 2 hr, and filtering.
Step 4: 200ml of an acidic solution having a pH of 1.5 was added to the residue and stirred for 15 minutes. This procedure was repeated three times.
Step 5:200ml of tap water was rinsed once. Tailings were obtained and the analytical results are shown in table 2.
TABLE 2 countercurrent leaching test results
From the table, the uranium leaching rate in the countercurrent test was 75.12%, while the thorium leaching rate was 35.27%.
2. Further extraction of thorium from tailings by alkali conversion
In order to improve the leaching rate of thorium, the countercurrent leaching tailings are subjected to alkali conversion treatment, so that sulfuric acid double salts of thorium in the slag are converted into hydroxide, and then dilute sulfuric acid treatment is carried out to further extract thorium. The method specifically comprises the following steps:
(1) Ammonium hydroxide dosage test
Step 1:100g of countercurrent leaching slag is taken, and the liquid-solid ratio is 1.2:1. ammonium hydroxide mass concentration is 25%, the dosage is 0.8ml, pH=8; 1ml, ph=9; 1.8ml, ph=10.
Step 2: stirring for 15 min, and discarding the filtrate.
Step 3: and adding sulfuric acid with the mass of 1% of the filter residue into the filter residue for acidification.
Step 4: the filtrate was filtered with acidified water three times with ph=1.5, 15 minutes of stirring each time, and no filtrate remained.
Step 5: the fourth time with tap water. Tailings were obtained and the analysis results are shown in table 3.
Table 3 ammonium hydroxide dosage test table
Note that: total leaching rate = (concentrate content-tailings content)/concentrate content
From this, ph=9 is optimal.
(2) Test of the amount of acidified sulfuric acid
The dosage of the acidified sulfuric acid is 5 percent and 10 percent of the mass of the countercurrent leaching slag respectively, and other conditions are the same as (1). The results are shown in Table 4.
TABLE 4 test table for the amount of acidified sulfuric acid
As can be seen from the table, the amount of sulfuric acid used in the acidification is preferably 5%.
(3) Alkali conversion time test
Ammonium hydroxide was added to make ph=9. Acidification with 5% sulfuric acid. The conversion time was divided into 15 minutes, 30 minutes and 1 hour, and the other conditions were the same as in (2). The results are shown in Table 5.
TABLE 5 alkaline conversion time test table
From the table, the conversion time was optimal for 15 minutes.
(III) expansion verification experiment
According to the selected test conditions, 19kg of the mixed concentrate subjected to magnetic separation is taken for expansion experiments, and the final tailings are subjected to 3 times of sampling analysis. The results are shown in Table 6.
TABLE 6 analysis of the results of countercurrent leaching tests
The uranium grade in the tailings is 0.0147%, and the thorium grade is 0.065%. The uranium leaching rate is 80.74 percent and the thorium leaching rate is 71.24 percent.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore, which is characterized by comprising the following steps:
step S1: grinding the green layer silicon-cerium titanium ore to obtain coarse ore with the thickness of-1-0 mm; wherein, coarse ore with the diameter of-0.074-0 mm is used as ore slurry to enter bulk concentrate;
feeding the coarse ore with the diameter of-1+0.074 mm into the next step of two-stage magnetic separation;
step S2: carrying out first-stage magnetic separation on coarse ore with the magnetic field strength of 10000-11000 Oerst and the coarse ore with the magnetic field strength of-1+0.074 mm, and taking the passed ore as concentrate to enter bulk concentrate;
carrying out second-stage magnetic separation on the non-passing ores by using a magnetic field with the intensity of 12000-13000 Oerst, wherein the passing part enters bulk concentrate, and the non-passing ores are tailings;
step S3: countercurrent leaching is carried out on the bulk concentrate, and uranium and thorium in the bulk concentrate are extracted;
the method specifically comprises the following steps: adding sulfuric acid, calcium fluoride and manganese dioxide into the bulk concentrate, stirring, fully reacting, adding water, sulfuric acid and manganese dioxide for secondary reaction, and filtering after the secondary reaction is finished; collecting filtrate;
adding an acidic solution into the obtained filter residues, stirring, and pulping for 2-5 times;
flushing leaching residues;
step S4: and (3) adding alkali into the leaching slag in the step (S3) for treatment, and then reacting with dilute sulfuric acid to extract thorium.
2. The method for extracting uranium and thorium from green-layer silicon-cerium-titanium ore according to claim 1, wherein in the step S2: and carrying out first-stage magnetic separation on the coarse ore with the magnetic field strength of 10500-10700 Oersted to obtain coarse ore with the magnetic field strength of-1+0.074 mm.
3. The method for extracting uranium and thorium from green-layer bastnaesite according to claim 1, wherein the grain size of the bulk concentrate is-0.417 mm to-0.074 mm.
4. The method for extracting uranium and thorium from green-layer cerite according to claim 1, wherein 22% sulfuric acid, 3% calcium fluoride, 1% manganese dioxide and a liquid-solid ratio of sulfuric acid to ore of 1.2 are added to 100g of bulk concentrate with a particle size of-0.208 mm based on mass of the bulk concentrate: 1, stirring and reacting for 2 hours at 120 ℃.
5. The process for extracting uranium and thorium from green-layer bastnaesite according to claim 1, wherein 200ml of water, 3% sulfuric acid, 1% manganese dioxide are added and the secondary reaction is carried out at 80 ℃ for 2 hours.
6. The method for extracting uranium and thorium from green-layer bastnaesite according to claim 1, wherein the step S4 specifically includes:
100g of ammonium hydroxide with the mass concentration of 25% is added into the leaching residue in the step S3, and the mixture is stirred and filtered after full reaction; collecting filtrate;
acidifying the filter residue with 0.5-1% sulfuric acid, washing with acidified water with pH value of 1.5 for 3-5 times, stirring for 15 min during each washing, and filtering; collecting filter residues;
the filter residue is rinsed with water, and the tailings are reserved.
7. The method according to claim 6, wherein in the step S4,
acidifying the filter residue with 0.5% sulfuric acid, washing with acidified water with pH value of 1.5 for 3-5 times, stirring for 15 min during each washing, and filtering; and (5) collecting filter residues.
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