CN101182601A - Method for extracting metal scandium and titanium from red mud - Google Patents
Method for extracting metal scandium and titanium from red mud Download PDFInfo
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- CN101182601A CN101182601A CNA2007101161528A CN200710116152A CN101182601A CN 101182601 A CN101182601 A CN 101182601A CN A2007101161528 A CNA2007101161528 A CN A2007101161528A CN 200710116152 A CN200710116152 A CN 200710116152A CN 101182601 A CN101182601 A CN 101182601A
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- scandium
- red mud
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- hydrochloric acid
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- 229910052706 scandium Inorganic materials 0.000 title claims abstract description 134
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims abstract description 134
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000010936 titanium Substances 0.000 title claims abstract description 23
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 102
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000000605 extraction Methods 0.000 claims abstract description 52
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052742 iron Inorganic materials 0.000 claims abstract description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- 238000002386 leaching Methods 0.000 claims abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- 239000011575 calcium Substances 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000007062 hydrolysis Effects 0.000 claims abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 239000012074 organic phase Substances 0.000 claims description 61
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000012535 impurity Substances 0.000 claims description 33
- 238000001914 filtration Methods 0.000 claims description 27
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- 238000005554 pickling Methods 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 239000003350 kerosene Substances 0.000 claims description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- -1 decyl tertiary amine Chemical class 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 230000004087 circulation Effects 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 239000011499 joint compound Substances 0.000 claims description 2
- 230000000877 morphologic effect Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 2
- 239000000413 hydrolysate Substances 0.000 abstract 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 6
- LQPWUWOODZHKKW-UHFFFAOYSA-K scandium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Sc+3] LQPWUWOODZHKKW-UHFFFAOYSA-K 0.000 description 6
- 239000011790 ferrous sulphate Substances 0.000 description 5
- 235000003891 ferrous sulphate Nutrition 0.000 description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000007654 immersion Methods 0.000 description 3
- KOQOJLXRPCIFKW-UHFFFAOYSA-N oxalic acid scandium Chemical compound [Sc].C(C(=O)O)(=O)O.[Sc] KOQOJLXRPCIFKW-UHFFFAOYSA-N 0.000 description 3
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for extracting metal scandium and titanium from red mud; the method is used for extracting scandium and titanium from the red mud; the method takes the red mud which is produced through the sinter process of the high-grade ore two portion of clinker in alumina plant as the raw material; the hydrochloric acid with a concentration of 2 percent to 6 percent is used for leaching the calcium and sodium from the red mud to increase the content of the scandium and titanium in the red mud; and then the hydrochloric acid with a concentration of 16 percent to 22 percent is used for a second acid dipping of the red mud and the product of scandium oxide is obtained after the leaching liquid passes the processes of extraction, reverse extraction and baking; the hydrochloric acid with a concentration of 80 percent to 90 percent is used for a third acid dipping of the red mud after the second one and the leaching liquid is added with iron powder for reduction and then the temperature is reduced to crystallize and separate out iron in the pattern of FeSO<4>.7H<2>O; the acid liquid which contains titanium after the iron is removed is added with alkali and heated for hydrolysis; the product of titanium oxide is obtained after the hydrolysate is baked. The method is simple and easy to be carried out and most metal elements in the red mud can be recovered and the cost for processing the red mud is low, all of which are beneficial to the comprehensive utilization of the red mud.
Description
Technical field
The present invention relates to a kind of method of from red mud, extracting metal scandium, titanium, be used for extracting the metal scandium and the metal titanium of red mud.
Background technology
At present, the method that existing red mud is carried scandium is the hydrochloric acid reaction with the red mud that produces in the aluminum oxide production process and 22～30%, obtains containing the leach liquor of scandium, extracts, step such as back extraction removal of impurities, purification again.The content of scandium is lower in the used raw material of this method, has only 0.0082%, make 1 kilogram of Scium trioxide and need handle 328 tons of red muds, the treatment capacity of red mud is bigger, and this method titanium that content in the red mud is higher is disposed as impurity, caused the waste of resource, the comprehensive utilization degree of red mud is low.
Summary of the invention
The object of the present invention is to provide a kind of method of from red mud, extracting metal scandium, titanium, simple and easy to do, make the metallic element in the red mud obtain higher recovery, reduced the red mud processing cost, be beneficial to the comprehensive utilization of red mud.
The method of from red mud, extracting metal scandium, titanium of the present invention, the red mud that produces with the rich ore two component grog firing process of alumina producer is a raw material, the hydrochloric acid of the ratio of the quality of aqueous hydrochloric acid (HCL with) leaches the sodium in the red mud, calcium at first to be 2～6% with concentration, the content of scandium and titanium in the red mud is improved, be that 16～22% the hydrochloric acid red mud after to an acidleach carries out secondary pickling with concentration then, leach liquor obtains the Scium trioxide product by extraction, back extraction, removal of impurities, roast operation; Be that 80%～90% the sulfuric acid red mud after to secondary pickling carries out three acidleach with concentration at last, leach liquor is lowered the temperature after adding iron powder reducing, makes iron with FeSO
4.7H
2The morphological crystal of O is separated out, and uses the distilled water wash crystallisate, must be after air-dry with the ferrous sulfate product of 7 crystal water, the titaniferous pickling liquor after the deironing adds the hydrolysis of alkali post-heating, behind the hydrolyzate roast titanium oxide product.Scandium is carried in a hydrolysising mother liquid extraction, to improve total extraction yield of Scium trioxide.
Wherein:
The leaching condition of sodium, calcium is: adding concentration is 2～6% hydrochloric acid in acid-proof reaction groove, add the rich ore red mud again, liquid-solid ratio is controlled to be (3～6): 1, temperature of reaction is 80～90 ℃, reacts 5～20 minutes, and the leaching yield of sodium oxide and calcium oxide is respectively greater than 85% and 50%, the red mud output capacity reaches 80%, after filtration, the content of Scium trioxide, titanium oxide rises to original 1.2 times in the red mud, and sodium, calcium are dissolved in the filtrate.
The extracting mode of scandium is:
(1) leaching of scandium: adding concentration is 16～22% hydrochloric acid in acid-proof reaction groove, adds the red mud after the acidleach again one time, and liquid-solid ratio is controlled to be 2.0～4.0, temperature of reaction is 90～98 ℃, reacted 20～60 minutes, and after filtration, must contain the leach liquor of scandium for (40～60) mg/L;
The extraction mode of scandium is:
1. with di(2-ethylhexyl)phosphate isooctyl (P204): kerosene is pressed (2～3): the proportional arrangement extraction agent of (97～98), with the leach liquor of this extraction agent and scandium by comparing O/A (organic phase and inorganic mutually volume ratio)=1: the mixed reaction of (8～10) obtains containing the scandium organic phase;
2. be 16～22% hydrochloric acid with concentration and contain scandium organic phase mixing, washing, remove the impurity that contains in the scandium organic phase, comparing O/A is 1: (1～3), mixing time are 5～10 minutes;
3. be that the NaOH of (1.0～3.0) mol/L is as reverse-extraction agent with concentration, with above-mentioned steps 2. gained contain scandium organic phase thorough mixing, compare O/A and be (1～3): 1, mixing time is 5～15 minutes, make scandium contained in the organic phase enter strip liquor, heating obtains scandium enriched substance: Sc (OH)
3Precipitation;
4. be 3. gained Sc (OH) of 16～22% hydrochloric acid macerate above-mentioned steps with concentration
3, the concentration that makes scandium in the solution is 600～800mg/L, gets Scium trioxide solution;
The purification mode of scandium is:
1. with extraction agent three sufferings/decyl tertiary amine (N235): kerosene is pressed (18～23): the proportional arrangement iron removing reagent of (77～82), this iron removing reagent and the above-mentioned Scium trioxide solution ratio in 1: 1 was mixed 5～15 minutes, impurity iron in the rich scandium solution is extracted in the organic phase, obtains the rich scandium solution after the deironing;
2. with extraction agent methyl-phosphorous acid diformazan heptyl ester (P350): kerosene is in (15～20): the ratio of (80～85) is configured, with the rich scandium solution after this organic phase and the deironing in 1: the ratio of (1～3) is carried out the secondary back extraction, obtains containing the scandium organic phase;
3. contain scandium organic phase 5～10 minute, partial impurities in removal organic phase for the hydrochloric acid of (6～8) mol/L by 1: 1 ratio washing with concentration;
4. with concentration be the NaOH of (5～7) mol/L as reverse-extraction agent, mixed back extraction 3～10 minutes with organic phase after the removal of impurities in 1: 1 ratio, the scandium in the organic phase is entered in the strip liquor, obtain the scandium enriched substance after the removal of impurities;
The preparation method of Scium trioxide:
Get rich scandium solution with hydrochloric acid macerate scandium enriched substance, the hydrochloric acid consumption is 5～8 times of hydrochloric acid macerate scandium enriched substance requirement, and concentration is 16～22%.Add ammoniacal liquor the pH value of rich scandium solution is transferred to 0.5～1.5, be heated to 80～100 ℃, adding solid oxalic acid reacts, 10～40 minutes after-filtration, after will filtering the washing of gained throw out, oven dry, put into stoving oven in 600～800 ℃ of roasting temperatures 1～2 hour, make purity greater than 98% Scium trioxide product.
The preparation method of titanium white is:
1. in the acid tolerance response jar, add concentration and be 80～90% sulfuric acid, add the red mud behind the secondary pickling again, liquid-solid ratio is controlled to be (1.2～3): 1, and temperature of reaction is 85～98 ℃, in 20～60 minutes reaction times, must contain the leach liquor of titanium oxide 40～90g/l after the filtration;
2. titaniferous leach liquor circulation is leached the red mud behind the secondary pickling, can 1～3 time, obtain high density titanium leach liquor, concentration adds reduced iron powder with the Fe in the solution greater than 100g/l
3+Be reduced into Fe
2+, the solution after the reduction is cooled to below 0 ℃, make iron with FeSO
47H
2The form crystallization of O is separated out, with 3～5 times 0 ℃ distilled water wash crystallisate, and must be after air-dry with the ferrous sulfate product of 7 crystal water.With the titaniferous pickling liquor hydro-oxidation sodium after the deironing, adjusting pH value is 1～3, being heated to boiling and being hydrolyzed, 3～4 hours after-filtration, the hydrate deposition (metatitanic acid) of titanium oxide;
3. with metatitanic acid earlier with the acidified water washing, use the triple distilled water wash with the place to go water-soluble impurity again, the oven dry back is in 700～1000 ℃ of roasting temperatures 1～2 hour, purity greater than 98% anatase type titanium oxide.
The present invention extracts the method for metal scandium, titanium from red mud, simple and easy to do, makes the metallic element in the red mud obtain higher recovery, has reduced the red mud processing cost, is beneficial to the comprehensive utilization of red mud.
Description of drawings
Fig. 1, process flow diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Producing of High-purity Sc Oxide:
At first the ratio that in liquid-solid ratio is 5.6: 1 with 4% hydrochloric acid and rich ore red mud is at 90 ℃ of 5 minutes after-filtration of reaction down, calculate the required concentrated hydrochloric acid and the water of hydrochloric acid of configuration 19% according to the moisture content in the filter cake, in liquid-solid ratio L/S=3: 1 ratio and filter cake must contain the leach liquor of scandium 52mg/L at 98 ℃ of 30 minutes after-filtration of reaction down.With di(2-ethylhexyl)phosphate isooctyl (P204): kerosene is by 1: 49 proportional arrangement extraction agent, with extraction agent with contain scandium solution by 1: 8 mixed reaction 10 minutes, obtain containing the scandium organic phase.Hydrochloric acid with 19% is that 1: 1 ratio washing contains the scandium organic phase 2 times in comparing O/A, washing time is 5 minutes/time, contain impurity such as part titanium in the scandium organic phase, iron with removal, be that the NaOH of 2.0mol/L is as reverse-extraction agent with concentration again, with the scandium organic phase that contains after the washing is 2: 1 mixed reaction 5 minutes by comparing O/A at normal temperatures, make the scandium in the organic phase enter strip liquor, obtain Sc (OH)
3Precipitation.
With concentration 19% hydrochloric acid macerate gained Sc (OH)
3, make the scandium concentration in the solution be about 600mg/L.With three sufferings/decyl tertiary amine (N235): kerosene was by 1: 4 proportional arrangement iron removing reagent, with iron removing reagent and rich scandium solution is 1: 1 mixed reaction 5 minutes by comparing O/A at room temperature, impurity iron in the rich scandium solution is extracted in the organic phase, obtains the rich scandium solution after the deironing.With methyl-phosphorous acid diformazan heptyl ester (P350): kerosene carries out secondary back extraction with the rich scandium solution after this organic phase and the deironing in 1: 1 ratio in 1: 4 ratio preparation, and the extraction time is 10 minutes/time, obtains containing the scandium organic phase.Hydrochloric acid with 7mol/L contained the scandium organic phase 5 minutes in the ratio washing that is in a ratio of 1: 1, remove the partial impurities in the organic phase, be that the NaOH of 6mol/L is as reverse-extraction agent with concentration again, reacted 10 minutes by the mixed that is in a ratio of 1: 1 with the scandium organic phase that contains after the removal of impurities, make the scandium in the organic phase enter strip liquor, obtain the scandium enriched substance after the removal of impurities.
With concentration is that 19% hydrochloric acid macerate scandium enriched substance gets rich scandium solution, the hydrochloric acid consumption is 6 times of hydrochloric acid macerate scandium enriched substance requirement, add ammoniacal liquor the pH value of rich scandium solution is transferred to 1.2, add the reaction of solid oxalic acid when being heated to 85 ℃, 20 minutes after-filtration, to filter gained throw out (oxalic acid scandium) and put into stoving oven after with 5 times distilled water washs, oven dry, in 800 ℃ of following roastings 1 hour purity is 98% Scium trioxide.
Producing of titanium white:
Adding concentration is 85% sulfuric acid in the acid tolerance response jar, add the red mud behind the secondary pickling again, the ratio that in liquid-solid ratio L/S is 2: 1 is at 98 ℃ of 0.5 hour after-filtration of reaction down, obtain containing the leach liquor of titanium oxide 65g/l, leach liquor is carried out 1 circulation again leach, obtain the leach liquor that titanium oxide concentration is 118g/l.According to Fe in the leach liquor
3+Concentration add an amount of reduced iron powder with Fe
3+Be reduced into Fe
2+, be cooled to-3 ℃ and make iron in the solution with FeSO
47H
2The form crystallization of O is separated out, with 4 times 0 ℃ distilled water wash crystallisate, and must be after air-dry with the ferrous sulfate product of 7 crystal water.Titaniferous pickling liquor after the deironing add NaOH with pH value transfer to 2 post-heating to the boiling be hydrolyzed, 4 hours after-filtration get the hydrate deposition (metatitanic acid) of titanium oxide.The gained metatitanic acid with 1% sulfuric acid dilute solution washing 2 times, washes with water 2 times earlier again, the place to go water-soluble impurity, and it is 98.26% anatase type titanium oxide that the oven dry back got purity in 1 hour in 900 ℃ of following roastings.
The hydrolysising mother liquid concentration of titanium oxide is that 10% di(2-ethylhexyl)phosphate isooctyl (P204) extracts and carries scandium, with the thick scandium hydroxide of gained after the alkali lye back extraction with purify again after the thick scandium hydroxide of gained from the quadratic acid immersion liquid mixes, to improve the extraction yield of Scium trioxide.
Embodiment 2
Producing of High-purity Sc Oxide:
At first the ratio that in liquid-solid ratio is 4: 1 with 6% hydrochloric acid and rich ore red mud is at 90 ℃ of 10 minutes after-filtration of reaction down, calculate the required concentrated hydrochloric acid and the water of hydrochloric acid of configuration 19% according to the moisture content in the filter cake, in liquid-solid ratio L/S=2.6: 1 ratio and filter cake must contain the leach liquor of scandium 59mg/L at 95 ℃ of 50 minutes after-filtration of reaction down.With di(2-ethylhexyl)phosphate isooctyl (P204): kerosene is by 1: 24 proportional arrangement extraction agent, with extraction agent with contain scandium solution by 1: 10 mixed reaction 10 minutes, obtain containing the scandium organic phase.Hydrochloric acid with 18% is that 1: 1 ratio washing contains the scandium organic phase 2 times in comparing O/A, washing time is 5 minutes/time, contain impurity such as part titanium in the scandium organic phase, iron with removal, be that the NaOH of 1.5mol/L is as reverse-extraction agent with concentration again, with the scandium organic phase that contains after the washing is 1: 1 mixed reaction 5 minutes by comparing O/A at normal temperatures, make the scandium in the organic phase enter strip liquor, obtain Sc (OH)
3Precipitation.
With concentration 20% hydrochloric acid macerate gained Sc (OH)
3, make the scandium concentration in the solution be about 650mg/L.With three sufferings/decyl tertiary amine (N235): kerosene was by 9: 41 proportional arrangement iron removing reagent, with iron removing reagent and rich scandium solution is 1: 1 mixed reaction 5 minutes by comparing O/A at room temperature, impurity iron in the rich scandium solution is extracted in the organic phase, obtains the rich scandium solution after the deironing.With methyl-phosphorous acid diformazan heptyl ester (P350): kerosene carries out secondary back extraction with the rich scandium solution after this organic phase and the deironing in 1: 1 ratio in 3: 17 ratio preparation, and the extraction time is 10 minutes/time, obtains containing the scandium organic phase.Salt acid elution with 6mol/L contained the scandium organic phase 8 minutes, remove the partial impurities in the organic phase, be that the NaOH of 5mol/L is as reverse-extraction agent with concentration again, reacted 10 minutes by the mixed that is in a ratio of 1: 1 with the scandium organic phase that contains after the removal of impurities, make the scandium in the organic phase enter strip liquor, obtain the scandium enriched substance after the removal of impurities.
With concentration is that 18% hydrochloric acid macerate scandium enriched substance gets rich scandium solution, the hydrochloric acid consumption is 7 times of hydrochloric acid macerate scandium enriched substance requirement, add ammoniacal liquor the pH value of rich scandium solution is transferred to 1.0, add the reaction of solid oxalic acid when being heated to 90 ℃, 30 minutes after-filtration, to filter gained throw out (oxalic acid scandium) and put into stoving oven after with 5 times distilled water washs, oven dry, in 800 ℃ of following roastings 1 hour purity is 98.37% Scium trioxide.
Producing of titanium white:
Adding concentration is 82% sulfuric acid in the acid tolerance response jar, add the red mud behind the secondary pickling again, the ratio that in liquid-solid ratio L/S is 3: 1 is at 98 ℃ of 0.5 hour after-filtration of reaction down, obtain containing the leach liquor of titanium oxide 44g/l, leach liquor is carried out 2 circulations again leach, obtain the leach liquor that titanium oxide concentration is 113g/l.According to Fe in the leach liquor
3+Concentration add an amount of reduced iron powder with Fe
3+Be reduced into Fe
2+, be cooled to-5 ℃ and make iron in the solution with FeSO
47H
2The form crystallization of O is separated out, with 4 times 0 ℃ distilled water wash crystallisate, and must be after air-dry with the ferrous sulfate product of 7 crystal water.Titaniferous pickling liquor after the deironing add NaOH with pH value transfer to 1 post-heating to the boiling be hydrolyzed, 4 hours after-filtration get the hydrate deposition (metatitanic acid) of titanium oxide.The gained metatitanic acid with 1% sulfuric acid dilute solution washing 2 times, washes with water 2 times earlier again, the place to go water-soluble impurity, and it is 98.35% anatase type titanium oxide that the oven dry back got purity in 1 hour in 850 ℃ of following roastings.
The hydrolysising mother liquid concentration of titanium oxide is that 10% di(2-ethylhexyl)phosphate isooctyl (P204) extracts and carries scandium, with the thick scandium hydroxide of gained after the alkali lye back extraction with purify again after the thick scandium hydroxide of gained from the quadratic acid immersion liquid mixes, to improve the extraction yield of Scium trioxide.
Embodiment 3
Producing of High-purity Sc Oxide:
At first the ratio that in liquid-solid ratio is 6: 1 with 5% hydrochloric acid and rich ore red mud is at 80 ℃ of 15 minutes after-filtration of reaction down, calculate the required concentrated hydrochloric acid and the water of hydrochloric acid of configuration 19% according to the moisture content in the filter cake, in liquid-solid ratio L/S=3.5: 1 ratio and filter cake must contain the leach liquor of scandium 45mg/L at 90 ℃ of 30 minutes after-filtration of reaction down.With di(2-ethylhexyl)phosphate isooctyl (P204): kerosene is by 1: 49 proportional arrangement extraction agent, with extraction agent with contain scandium solution by 1: 8 mixed reaction 10 minutes, obtain containing the scandium organic phase.Hydrochloric acid with 21% is that 1: 1 ratio washing contains the scandium organic phase 2 times in comparing O/A, washing time is 5 minutes/time, contain impurity such as part titanium in the scandium organic phase, iron with removal, be that the NaOH of 3.0mol/L is as reverse-extraction agent with concentration again, is 3: 1 ratio hybrid reaction 10 minutes at normal temperatures with the scandium organic phase that contains after the washing in comparing O/A, make the scandium in the organic phase enter strip liquor, obtain Sc (OH)
3Precipitation.
With concentration 20% hydrochloric acid macerate gained Sc (OH)
3, make the scandium concentration in the solution be about 600mg/L.With three sufferings/decyl tertiary amine (N235): kerosene was by 23: 77 proportional arrangement iron removing reagent, iron removing reagent and rich scandium solution were at room temperature reacted 10 minutes by the mixed that is in a ratio of 1: 1, impurity iron in the rich scandium solution is extracted in the organic phase, obtains the rich scandium solution after the deironing.With methyl-phosphorous acid diformazan heptyl ester (P350): kerosene carries out secondary back extraction with the rich scandium solution after this organic phase and the deironing in 1: 1 ratio in 1: 4 ratio preparation, and the extraction time is 10 minutes/time, obtains containing the scandium organic phase.Hydrochloric acid with 8mol/L contained the scandium organic phase 10 minutes in the ratio washing of comparing 1: 1, remove the partial impurities in the organic phase, be that the NaOH of 6.5mol/L is as reverse-extraction agent with concentration again, reacted 10 minutes by the mixed that is in a ratio of 1: 1 with the scandium organic phase that contains after the removal of impurities, make the scandium in the organic phase enter strip liquor, obtain the scandium enriched substance after the removal of impurities.
With concentration is that 20% hydrochloric acid macerate scandium enriched substance gets rich scandium solution, the hydrochloric acid consumption is 7 times of hydrochloric acid macerate scandium enriched substance requirement, add ammoniacal liquor the pH value of rich scandium solution is transferred to 1.1, add the reaction of solid oxalic acid when being heated to 90 ℃, 20 minutes after-filtration, to filter gained throw out (oxalic acid scandium) and put into stoving oven after with 5 times distilled water washs, oven dry, in 800 ℃ of following roastings 1 hour purity is 98.69% Scium trioxide.
Producing of titanium white:
Adding concentration is 90% sulfuric acid in the acid tolerance response jar, add the red mud behind the secondary pickling again, the ratio that in liquid-solid ratio L/S is 1.5: 1 is at 98 ℃ of 0.5 hour after-filtration of reaction down, obtain containing the leach liquor of titanium oxide 76g/l, leach liquor is carried out 1 circulation again leach, obtain the leach liquor that titanium oxide concentration is 137g/l.According to Fe in the leach liquor
3+Concentration add an amount of reduced iron powder with Fe
3+Be reduced into Fe
2+, be cooled to-5 ℃ and make iron in the solution with FeSO
47H
2The form crystallization of O is separated out, with 4 times 0 ℃ distilled water wash crystallisate, and must be after air-dry with the ferrous sulfate product of 7 crystal water.Titaniferous pickling liquor after the deironing add NaOH with pH value transfer to 1.5 post-heating to the boiling be hydrolyzed, 4 hours after-filtration get the hydrate deposition (metatitanic acid) of titanium oxide.The gained metatitanic acid with 1% sulfuric acid dilute solution washing 2 times, washes with water 2 times earlier again, the place to go water-soluble impurity, and it is 98.75% anatase type titanium oxide that the oven dry back got purity in 1 hour in 950 ℃ of following roastings.
The hydrolysising mother liquid concentration of titanium oxide is that 10% di(2-ethylhexyl)phosphate isooctyl (P204) extracts and carries scandium, with the thick scandium hydroxide of gained after the alkali lye back extraction with purify again after the thick scandium hydroxide of gained from the quadratic acid immersion liquid mixes, to improve the extraction yield of Scium trioxide.
Claims (4)
1. method of from red mud, extracting metal scandium, titanium, it is characterized in that the red mud that produces with the rich ore two component grog firing process of alumina producer is a raw material, be that 2～6% hydrochloric acid leaches the sodium in the red mud, calcium at first with concentration, the content of scandium and titanium in the red mud is improved, be that 16～22% the hydrochloric acid red mud after to an acidleach carries out secondary pickling with concentration then, leach liquor obtains the Scium trioxide product by operations such as extraction, back extraction, removal of impurities, roasts; Be that 80%～90% the sulfuric acid red mud after to secondary pickling carries out three acidleach with concentration at last, leach liquor is lowered the temperature after adding iron powder reducing, makes iron with FeSO
4.7H
2The morphological crystal of O is separated out, and the titaniferous pickling liquor after the deironing adds the hydrolysis of alkali post-heating, gets titanium oxide product behind the hydrolyzate roast.
2. the method for from red mud, extracting metal scandium, titanium according to claim 1, the leaching condition that it is characterized in that sodium, calcium: adding concentration is 2～6% hydrochloric acid in acid-proof reaction groove, add the rich ore red mud again, liquid-solid ratio is controlled to be (3～6): 1, temperature of reaction is 80～90 ℃, reacts 5～20 minutes, after filtration, the content of Scium trioxide, titanium oxide rises to original 1.2 times in the red mud, and sodium, calcium are dissolved in the filtrate.
3. the method for extracting metal scandium, titanium from red mud according to claim 2 is characterized in that the extraction of scandium:
(1) leaching of scandium: adding concentration is 16～22% hydrochloric acid in acid-proof reaction groove, adds the red mud after the acidleach again one time, and liquid-solid ratio is controlled to be 2.0～4.0, temperature of reaction is 90～98 ℃, reacted 20～60 minutes, and after filtration, must contain the leach liquor of scandium for (40～60) mg/L;
(2) extraction of scandium:
1. with the di(2-ethylhexyl)phosphate isooctyl: kerosene is by (2～3): the proportional arrangement extraction agent of (97～98), with the leach liquor of this extraction agent and scandium by comparing O/A=1: the mixed reaction of (8～10) 5～15 minutes obtains containing the scandium organic phase;
2. be 16～22% hydrochloric acid with concentration and contain scandium organic phase mixing, washing, remove the impurity that contains in the scandium organic phase, comparing O/A is 1: (1～3), mixing time are 5～10 minutes;
3. be that the NaOH of (1.0～3.0) mol/L is as reverse-extraction agent with concentration, with above-mentioned steps 2. gained contain scandium organic phase thorough mixing, compare O/A and be (1～3): 1, mixing time is 5～15 minutes, make scandium contained in the organic phase enter strip liquor, heating obtains scandium enriched substance: Sc (OH)
3Precipitation;
4. be 3. gained Sc (OH) of 16～22% hydrochloric acid macerate above-mentioned steps with concentration
3, the concentration that makes scandium in the solution is 600～800mg/L, gets Scium trioxide solution;
(3) purification of scandium:
1. with extraction agent three sufferings/decyl tertiary amine: kerosene is pressed (18～23): the proportional arrangement iron removing reagent of (77～82), this iron removing reagent and the above-mentioned Scium trioxide solution ratio in 1: 1 was mixed 5～15 minutes, impurity iron in the rich scandium solution is extracted in the organic phase, obtains the rich scandium solution after the deironing;
2. with extraction agent methyl-phosphorous acid diformazan heptyl ester: kerosene is in (15～20): the ratio of (80～85) is configured, with the rich scandium solution after this organic phase and the deironing in 1: the ratio of (1～3) is carried out the secondary back extraction, obtains containing the scandium organic phase;
3. contain scandium organic phase 5～10 minute, partial impurities in removal organic phase for the hydrochloric acid of (6～8) mol/L by 1: 1 ratio washing with concentration;
4. with concentration be the NaOH of (5～7) mol/L as reverse-extraction agent, mixed back extraction 3～10 minutes with organic phase after the removal of impurities in 1: 1 ratio, the scandium in the organic phase is entered in the strip liquor, obtain the scandium enriched substance after the removal of impurities;
(4) producing of Scium trioxide:
Get rich scandium solution with hydrochloric acid macerate scandium enriched substance, the hydrochloric acid consumption is 5～8 times of hydrochloric acid macerate scandium enriched substance requirement, and concentration is 16～22%.Add ammoniacal liquor the pH value of rich scandium solution is transferred to 0.5～1.5, be heated to 80～100 ℃, add solid oxalic acid and react, 10～40 minutes after-filtration, after will filtering gained throw out washing, oven dry,, make the Scium trioxide product in 600～800 ℃ of roasting temperatures 1～2 hour.
4. according to claim 1, the 2 and 3 described methods of from red mud, extracting metal scandium, titanium, it is characterized in that producing of titanium white:
1. add concentration and be 80～90% sulfuric acid in the acid tolerance response jar, add the red mud behind the secondary pickling again, liquid-solid ratio is controlled to be (1.2～3): 1, temperature of reaction is 85～98 ℃, 20～60 minutes reaction times, after the filtration the titaniferous leach liquor;
2. titaniferous leach liquor circulation is leached the red mud behind the secondary pickling, obtains high density titanium leach liquor, add reduced iron powder reduction back cooling, with iron with FeSO
47H
2The form crystallization of O is separated out, and with the titaniferous pickling liquor hydro-oxidation sodium after the deironing, adjusting pH value is 1～3, being heated to boiling and being hydrolyzed, 3～4 hours after-filtration, the hydrate deposition of titanium oxide;
3. with metatitanic acid earlier with the acidified water washing, use distilled water wash again, the oven dry back is in 700～1000 ℃ of roasting temperatures 1～2 hour, the anatase type titanium oxide product.
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