CN111748701A - Direct leaching process for titanium recovery sulfuric acid - Google Patents
Direct leaching process for titanium recovery sulfuric acid Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 187
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000010936 titanium Substances 0.000 title claims abstract description 39
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000011084 recovery Methods 0.000 title claims description 14
- 239000002893 slag Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000010419 fine particle Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 abstract description 15
- 229910052742 iron Inorganic materials 0.000 abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 22
- 229910052593 corundum Inorganic materials 0.000 description 22
- 229910001845 yogo sapphire Inorganic materials 0.000 description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 239000002253 acid Substances 0.000 description 12
- 238000004064 recycling Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910052595 hematite Inorganic materials 0.000 description 5
- 239000011019 hematite Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 4
- 229910052622 kaolinite Inorganic materials 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- -1 rectorite Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
- C22B34/125—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors containing a sulfur ion as active agent
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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Abstract
The invention discloses a direct leaching process for recovering sulfuric acid from titanium, which comprises the following steps: (1) grinding raw ore to fine particles; (2) adding the ground raw ore and a sulfuric acid solution into a leacher, heating to boil, and performing first-stage leaching to obtain first-stage ore pulp; (3) filtering the first-stage ore pulp to obtain first-stage leaching slag and first-stage leaching liquid; (4) adding the first-stage leaching residue and a sulfuric acid solution into a leacher, heating to boil, and performing second-stage leaching to obtain second-stage ore pulp; (5) and filtering the second-stage ore pulp to obtain second-stage leaching slag and second-stage leaching liquid. After the first-stage leaching and the second-stage leaching, the total leaching rate of iron is 99.69%, the total leaching rate of titanium is 91.55%, and the total leaching rate of aluminum is 98.84%.
Description
Technical Field
The invention belongs to the technical field of titanium recovery in raw ores, and particularly relates to a direct leaching process for recovering sulfuric acid from titanium.
Background
TiO is the main valuable component in the sedimentary ore2Mainly exists in anatase, and the particle size of anatase is-30 μm. The gangue minerals are mainly hematite, quartz, kaolinite and rectorite. Kaolinite and rectorite are aluminum carrier minerals, the particles of which are fine, are in a fine dispersion state and are distributed in a cryptocrystalline aggregate, and the surfaces of the kaolinite and the rectorite are turbid; the hematite and limonite are in a fine dispersion state, the granularity of the hematite and limonite is about 2 mu m, and the hematite and the limonite are locally distributed as a lump aggregate; the quartz is fine microcrystal and exists in a fine granular monomer or irregular aggregate shape, the particle size of the monomer is about 2-8 mu m, the distribution is not uniform, and the quartz is mostly filled in the pore space of the ore. The primary mineral particle size is so fine and dispersed that effective separation and recovery of anatase is difficult with conventional physical beneficiation processes. Therefore, the invention provides a chemical beneficiation (chemical leaching) process for recycling titanium.
Disclosure of Invention
The invention provides a direct leaching process for recovering sulfuric acid from titanium, which aims to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a direct leaching process of titanium recovery sulfuric acid comprises the following steps:
s1: grinding raw ore to fine particles;
s2: adding the ground raw ore and a sulfuric acid solution into a leacher, heating to boil, and performing first-stage leaching to obtain first-stage ore pulp;
s3: filtering the first-stage ore pulp to obtain first-stage leaching slag and first-stage leaching liquid;
s4: adding the first-stage leaching residue and a sulfuric acid solution into a leacher, heating to boil, and performing second-stage leaching to obtain second-stage ore pulp;
s5: and filtering the second-stage ore pulp to obtain second-stage leaching slag and second-stage leaching liquid.
As a further description of the above technical solution: the raw ore ground to-0.075 mm in the step S1 accounts for 65-95%.
As a further description of the above technical solution: the concentration of the sulfuric acid solution in the step S2 is 40-80% (volume concentration).
As a further description of the above technical solution: the leaching time in the step S2 is 60-150 min.
As a further description of the above technical solution: the solid ratio of the leaching solution in the step S2 is 4-6.
As a further description of the above technical solution: the leaching temperature in the step S2 is 140 °.
As a further description of the above technical solution: the step S3 specifically includes: and cooling the first-stage ore pulp to 90 ℃, and filtering to obtain first-stage leaching residue.
As a further description of the above technical solution: the concentration of the sulfuric acid solution in the step S4 is 85 to 95% (volume concentration).
As a further description of the above technical solution: the leaching time in the step S4 is 90-150 min.
As a further description of the above technical solution: the solid ratio of the leaching solution in the step S4 is 3-4.
As a further description of the above technical solution: the leaching temperature in the step S4 is 250 °.
As a further description of the above technical solution: the step S5 specifically includes: and cooling the second-stage ore pulp to 90 ℃, and filtering to obtain second-stage leaching residues.
As a further description of the above technical solution: the process also comprises adding the second-stage leachate to the leacher in the step S2, heating to boiling and carrying out the first-stage leaching.
As a further description of the above technical solution: the grinding equipment adopted in the step S1 is an XMB-70 three-roller four-cylinder rod mill.
As a further description of the above technical solution: the leachers in the steps S2 and S4 are mechanical agitation leachers.
As a further description of the above technical solution: the steps S2 and S4 are heated to boiling using an electric furnace.
As a further description of the above technical solution: and the steps S3 and S5 adopt a DZ-5C vacuum filter for filtration.
As a further description of the above technical solution: and drying the first-stage leaching residue and the second-stage leaching residue obtained in the steps S3 and S5 respectively by adopting an HG101-3 electrothermal blowing drying box.
The invention has the following beneficial effects:
1. after the first-stage leaching and the second-stage leaching, the total leaching rate of iron is 99.69%, the total leaching rate of titanium is 91.55%, and the total leaching rate of aluminum is 98.84%.
2. The test that the second-stage leachate returns to the first-stage leaching shows that the leaching effect is equivalent to that of the new acid with the same concentration, the second-stage acid can return to the first-stage leaching for recycling, the process flow of the Yaan anatase two-stage countercurrent leaching is determined through the research of the first-stage leaching and the second-stage leaching, and the technical indexes that the total leaching rate of iron is 99.70%, the total leaching rate of titanium is 91.42% and the total leaching rate of aluminum is 98.79% are obtained.
3. The leaching solution containing H2SO4398.27g/L, Al2O339.89g/L and TiO27.15g/L, TFe 27.73.73 g/L can be obtained by two-stage countercurrent leaching, and can be used for recycling iron, aluminum and titanium.
4. The two-stage countercurrent leaching process can obtain final leached slag containing SiO287.50%, Al2O30.84%, TFe 0.18%, TiO21.73%, CaO 0.02%, MgO 0.012% and loss on ignition 10%, and the slag powder may be used as reinforcing agent for concrete, water glass and other material.
Drawings
FIG. 1 is a flow chart of a direct leaching process for recovering sulfuric acid from titanium provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The raw ore mainly comprises hematite, kaolinite, rectorite, quartz and anatase, and the mineral contents of the raw ore are 30.63%, 18.63%, 15.12%, 14.74% and 5.46% respectively. The exploration test result shows that iron and aluminum in the ore are easier to leach than titanium, and if the leaching rate of titanium is high at one time, the sulfuric acid concentration and the leaching time of sulfuric acid leaching need to be increased, which inevitably increases the leaching cost. For this purpose, the test considers the study of the process conditions by means of a two-stage leaching process. The aim is to consider the leaching of iron and aluminium first in the first stage and to concentrate the leaching of titanium in the second stage.
As shown in fig. 1, a direct leaching process of sulfuric acid recovered from titanium comprises:
(1) the raw ore is ground to fine particles.
(2) Adding the ground raw ore and a sulfuric acid solution into a leacher, heating to boil, and carrying out first-stage leaching to obtain first-stage ore pulp.
(3) And filtering the first-stage ore pulp to obtain first-stage leaching slag and first-stage leaching liquid.
(4) And adding the first-stage leaching residue and the sulfuric acid solution into a leacher, heating to boil, and performing second-stage leaching to obtain second-stage ore pulp.
(5) And filtering the second-stage ore pulp to obtain second-stage leaching slag and second-stage leaching liquid.
(6) And (3) adding the second-stage leachate into the leacher in the step (2), heating to boil, and performing first-stage leaching to realize recycling.
In the embodiment, raw ore ground to-0.075 mm in the step (1) accounts for 65-95%; the concentration of the sulfuric acid solution in the step (2) is 40-80% (volume concentration); the leaching time in the step (2) is 60-150 min; the solid-to-liquid ratio of the leaching solution in the step (2) is 4-6; the leaching temperature in the step (2) is 140 degrees.
In this embodiment, the concentration of the sulfuric acid solution in the step (4) is 85-95% (volume concentration); the leaching time in the step (4) is 90-150 min; the solid-to-liquid ratio of the leaching solution in the step (4) is 3-4; the leaching temperature in the step S4 is 250 °.
In this embodiment, the steps (1) and (2) are specifically: 1000g of raw ore is fed, raw ore with the grain size of-2 mm is ground to 85% of-0.075 mm, the sulfuric acid concentration is 50%, the liquid-solid ratio is 5:1, the leaching time is 120min, and the leaching temperature is 140 ℃. Obtaining first-stage leaching residue: TiO2214.13％、SiO276.36％、Al2O33.75%, TFe 1.40%, slag leaching rate: TiO228.42％、SiO23.96％、Al2O392.97 percent and TFe97.03 percent, and the yield of the leached residue is 40.12 percent. Mixing the first-stage leaching solution with a washing solution: TiO221.04g/L、SiO22.01g/L、Al2O345.02g/L, TFe 33.43.43 g/L, and the total volume of the solution is 5.75L. The first stage leaching mainly comprises leaching iron and aluminum in ores, and the produced leaching slag has low aluminum and iron contents, so that favorable conditions are created for leaching titanium in the next step.
In this embodiment, the step (3) is specifically: and cooling the first-stage ore pulp to 90 ℃, and filtering to obtain first-stage leaching residue.
In this embodiment, the step (4) specifically includes: 1000g of feed, 95 percent of sulfuric acid concentration and 3 percent of leaching solution solid ratio are heated to boiling leaching (250 ℃), and the leaching time is 120 min. Obtaining second-stage leaching residue: TiO221.71％、Al2O30.81%, TFe0.19%, total leaching rate: TiO2291.55％、Al2O398.84 percent, TFe 99.69 percent and the operation yield of the leached slag is 76.25 percent. Mixing the second-stage leaching solution with a washing solution: TiO2223.13g/L、Al2O36.94g/L, TFe 2.24.24 g/L, and the total volume of the solution is 2.04L. In this embodiment, the step (5) specifically includes: and cooling the second-stage ore pulp to 90 ℃, and filtering to obtain second-stage leaching residues.
In this embodiment, the step (6) adds the second-stage leachate to the leacher in the step (2), and heats the second-stage leachate to boiling for the first-stage leaching.
After the raw ore is leached by two stages, most of the titanium-iron-aluminum components are dissolved out, and particularly, the leaching rate of the titanium which is difficult to dissolve in acid is over 90 percent under the condition of two stages of high acid. However, the acidity of the leachate obtained by the second-stage leaching is high, and the leachate contains iron, titanium and aluminum, so that the leachate is convenient to comprehensively utilize, the leachate obtained by the second-stage leaching is returned to the first-stage leaching for leaching, whether the consumption of the neo-acid obtained by the first-stage leaching can be reduced is examined, and the similar leaching index is achieved.
The test was run at 1000g feed and the other test conditions were as before. The yield of the first-stage leaching residue of the recycled acid is 40.25 percent, and the contents of the leaching residues are respectively as follows: TiO2214.21％、Al2O33.72%, TFe 1.37%; the leaching rates of the slag meter are respectively as follows: TiO227.60％、Al2O393.00% and TFe 97.08%. The yield of the first-stage leaching residue of the new acid is 40.12 percent, and the contents of the leaching residues are respectively as follows: TiO2214.13％、Al2O33.75%, TFe 1.40%; the leaching rates of the slag meter are respectively as follows: TiO228.42％、Al2O392.97%, TFe97.03%; the contents of the recycled acid first-stage leaching solution and the washing solution after mixing are respectively as follows: h2SO4398.72g/L、TiO27.15g/L、TFe 27.73g/L、Al2O339.89g/L, and the total volume of the solution is 7.40L. After the first stage leaching operation adopts second-stage acid for recycling leaching, the leaching indexes of iron, aluminum and titanium are equivalent to the leaching result of the new acid, so that the second-stage leaching solution can be returned to the first stage for use.
In the embodiment, the grinding equipment adopted in the step (1) is an XMB-70 three-roller four-cylinder rod mill; the leacher in the steps (2) and (4) is a mechanical stirring leacher; heating the steps (2) and (4) to boiling by using an electric furnace; filtering in the steps (3) and (5) by adopting a DZ-5C vacuum filter; and (4) drying the first-stage leached residues and the second-stage leached residues obtained in the steps (3) and (5) by adopting an HG101-3 electrothermal blowing drying box.
The Yaan Yanxi channel titanium ore recycling process is a two-section countercurrent sulfuric acid leaching process. The technological process is shown in figure 1, the technical parameters of the leaching process are as follows: raw ore with the feeding fineness of-0.075 mm accounts for more than 85% of the total raw ore, the sulfuric acid concentration is 50%, the liquid-solid ratio is 5:1, the leaching temperature is 140 ℃, and the leaching time is 120 min; the conditions of the second stage leaching are as follows: the concentration of sulfuric acid is 95%, the liquid-solid ratio is 3:1, the leaching temperature is 250 ℃, and the leaching time is 120 min. The contents of the first-stage leaching residues are respectively as follows: TiO2214.21％、Al2O33.72%, TFe 1.37%; the corresponding leaching rates are respectively as follows: TiO227.60％、Al2O393.00%, TFe 97.08%; the contents of the second-stage leaching residues are respectively as follows: TiO221.73％、Al2O30.84%, TFe 0.18%; the corresponding leaching rates are respectively as follows: TiO2290.72％、Al2O382.78%, TFe 89.98%; the total leaching rates are respectively: TiO2291.42％、Al2O398.79% and TFe99.70%. The content of the mixed leaching solution and the washing solution is respectively as follows: h2SO4398.72g/L、TiO27.15g/L、TFe27.73g/L、Al2O339.89g/L, and the total volume of the solution is 7.40L. The content of main elements in the leaching residue is shown in a table 1-1, and the measurement result of part of physical property parameters of the micro powder of the finally leached residue after grinding is shown in a table 1-2. The main mineral of the final leaching residue of Yaan Yanxi channel titanium ore is silicon dioxide, and the micro powder of the milled leaching residue is 7d, active silicon dioxide with the activity index of 95 percent, and the slag powder can be used as a concrete reinforcing agent and a raw material for producing water glass and the like.
TABLE 1-1 Yaan Yanxi channel titanium mine final leaching residue multielement analysis result
| Principal Components | TiO2 | Al2O3 | TFe | SiO2 |
| Content (%) | 1.73 | 0.84 | 0.18 | 87.50 |
| Principal Components | CaO | MgO | K2O | Loss on ignition |
| Content (%) | 0.02 | 0.012 | 0.094 | 10 |
TABLE 1-2 measurement results of some physical property parameters of the final leached slag micropowder of Yaan Yanxi channel titanium mine
1. The invention determines the optimal process conditions of the first stage leaching as follows through a detailed first stage leaching condition test: grinding fineness of-0.075 mm accounts for 85.00%, sulfuric acid concentration is 50%, leaching solution solid ratio is 5, leaching time is 120min, and leaching temperature is 140 ℃. Under the optimal condition, the leaching rate of iron is 97.08 percent, the leaching rate of titanium is 7.60 percent, and the leaching rate of aluminum is 93.00 percent; the slag contains 1.37 percent of TFe and TiO214.13％、Al2O33.72% of good index.
2. The invention determines the optimal conditions of the second stage leaching to be as follows through a detailed second stage leaching condition test: the concentration of sulfuric acid is 95%, the liquid-solid ratio is 3, the leaching time is 120min, and the leaching temperature is 250 ℃. Under the best condition, the total leaching rate of iron is 99.69 percent, the total leaching rate of titanium is 91.55 percent, the total leaching rate of aluminum is 98.84 percent, and the second-stage slag contains 0.19 percent of TFe and 0.19 percent of TiO21.71％、Al2O3Good index of 0.81%.
3. The test that the second-stage leaching solution returns to the first-stage leaching shows that the leaching effect is equivalent to that of the new acid with the same concentration, which indicates that the second-stage acid can return to the first-stage leaching for recycling, and through the research of the first-stage leaching and the second-stage leaching, the process flow of the Yaan anatase two-stage countercurrent leaching is determined, and the technical indexes of 99.70% of the total leaching rate of iron, 91.42% of the total leaching rate of titanium and 98.79% of the total leaching rate of aluminum are obtained.
4. H can be obtained by two-stage countercurrent leaching2SO4398.27g/L、Al2O339.89g/L、TiO27.15g/L and TFe27.73g/L of leachate, which can be used for recycling iron, aluminum and titanium.
5. SiO-containing material can be obtained by two-stage countercurrent leaching287.50％、Al2O30.84％、TFe 0.18％、TiO21.73 percent of CaO, 0.02 percent of MgO, 0.012 percent of MgO and 10 percent of loss on ignition of the final leaching slagThe ground micropowder has volume average particle size of 7.31 μm, surface area average particle size of 2.61 μm, and specific surface area of 951.9m2The slag powder can be used as a concrete reinforcing agent and a raw material for producing water glass and the like.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A direct leaching process of sulfuric acid recovered from titanium is characterized by comprising the following steps:
s1: grinding raw ore to fine particles;
s2: adding the ground raw ore and a sulfuric acid solution into a leacher, heating to boil, and performing first-stage leaching to obtain first-stage ore pulp;
s3: filtering the first-stage ore pulp to obtain first-stage leaching slag and first-stage leaching liquid;
s4: adding the first-stage leaching residue and a sulfuric acid solution into a leacher, heating to boil, and performing second-stage leaching to obtain second-stage ore pulp;
s5: and filtering the second-stage ore pulp to obtain second-stage leaching slag and second-stage leaching liquid.
2. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the raw ore ground to-0.075 mm in the step S1 accounts for 65-95%.
3. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the concentration of the sulfuric acid solution in the step S2 is 40-80%; the leaching time in the step S2 is 60-150 min; the solid ratio of the leaching solution in the step S2 is 4-6.
4. The direct leaching process of sulfuric acid for titanium recovery according to claim 3, characterized in that: the leaching temperature in the step S2 is 140 °.
5. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the step S3 specifically includes: and cooling the first-stage ore pulp to 90 ℃, and filtering to obtain first-stage leaching residue.
6. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the concentration of the sulfuric acid solution in the step S4 is 85-95%; the leaching time in the step S4 is 90-150 min; the solid ratio of the leaching solution in the step S4 is 3-4.
7. The direct leaching process of sulfuric acid for titanium recovery according to claim 6, characterized in that: the leaching temperature in the step S4 is 250 °.
8. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the step S5 specifically includes: and cooling the second-stage ore pulp to 90 ℃, and filtering to obtain second-stage leaching residues.
9. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the process also comprises adding the second-stage leachate to the leacher in the step S2, heating to boiling and carrying out the first-stage leaching.
10. The direct leaching process of sulfuric acid for titanium recovery according to claim 1, characterized in that: the grinding equipment adopted in the step S1 is an XMB-70 three-roller four-cylinder rod grinder; the leachers in the steps S2 and S4 are mechanical agitation leachers; the steps S2 and S4 are heated to boiling by an electric furnace; filtering in the steps S3 and S5 by adopting a DZ-5C vacuum filter; and drying the first-stage leaching residue and the second-stage leaching residue obtained in the steps S3 and S5 respectively by adopting an HG101-3 electrothermal blowing drying box.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236816A (en) * | 1999-04-30 | 1999-12-01 | 中南工业大学 | Technology for comprehensive utilization of V-Ti magnetite |
| US20070092416A1 (en) * | 2005-10-18 | 2007-04-26 | Smith Earl M Jr | Titaniferous ore beneficiation |
| CN103276207A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium solution by wet-processing on vanadium-titanium magnetite concentrates |
| CN108165741A (en) * | 2018-01-23 | 2018-06-15 | 中国科学院过程工程研究所 | A kind of method that full acid system leaches metallic element in vanadium titano-magnetite |
| CN110453093A (en) * | 2019-09-11 | 2019-11-15 | 中南大学 | A kind of method of Ti-containing slag Selectively leaching titanium |
-
2020
- 2020-07-09 CN CN202010654960.5A patent/CN111748701B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236816A (en) * | 1999-04-30 | 1999-12-01 | 中南工业大学 | Technology for comprehensive utilization of V-Ti magnetite |
| US20070092416A1 (en) * | 2005-10-18 | 2007-04-26 | Smith Earl M Jr | Titaniferous ore beneficiation |
| CN103276207A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium solution by wet-processing on vanadium-titanium magnetite concentrates |
| CN108165741A (en) * | 2018-01-23 | 2018-06-15 | 中国科学院过程工程研究所 | A kind of method that full acid system leaches metallic element in vanadium titano-magnetite |
| CN110453093A (en) * | 2019-09-11 | 2019-11-15 | 中南大学 | A kind of method of Ti-containing slag Selectively leaching titanium |
Non-Patent Citations (1)
| Title |
|---|
| 陈龙: "《富钪锐钛矿原矿中钪的硫酸浸出试验及机理研究》", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 * |
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