CN104743606B - Metatitanic acid purification process - Google Patents
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- 239000002253 acid Substances 0.000 title claims abstract description 99
- 238000000746 purification Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 238000005342 ion exchange Methods 0.000 claims abstract description 18
- 238000005554 pickling Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 12
- 235000021110 pickles Nutrition 0.000 claims abstract description 10
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 7
- 238000004062 sedimentation Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 5
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 55
- 238000003756 stirring Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000003729 cation exchange resin Substances 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 29
- 239000004408 titanium dioxide Substances 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 5
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 abstract description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 11
- 238000004061 bleaching Methods 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229940072033 potash Drugs 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- 229910002703 Al K Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 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
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present patent application provides a kind of metatitanic acid purification process, the method be contain impurity metal ion metatitanic acid successively through pickle pickling, sedimentation and ion-exchange, return to again the continuous-flow cycle for the treatment of process of pickling, metatitanic acid in sedimentation backflows to pickling, supernatant flows and introduces ion-exchange step, carry out ion-exchange in ion exchange column, cyclic process is not less than 3 hours, after cyclic process finishes, the metatitanic acid of filter acid cleaning of evaporator lower floor, through routine washing, dehydration, obtain purifying metatitanic acid again. The technical program technique is simple, be easy to realize, pickle does not consume substantially, energy consumption is low, water consumption is few, and final purifying metatitanic acid can be for the preparation of downstream product such as high-quality titanium dioxide, Nano titanium dioxide, titanium sulfate, titanyl sulfates.
Description
Technical field
Patent application of the present invention relates to metatitanic acid purification method, in particular metal impurities is separated from metatitanic acidOut, make metatitanic acid be able to pure process.
Background technology
Metatitanic acid is the intermediate product of a core procedure in titanium dioxide manufacturing process. The predominant methods of preparing titanium dioxide is sulphurAcid system, the method, taking ilmenite as raw material, obtains titanium liquid through sulfuric acid solution, and titanium liquid makes hydrated titanium dioxide through hydrolysis again,Intermediate product metatitanic acid, metatitanic acid makes titanium dioxide through high-temperature calcination again. The preparation of metatitanic acid is the core of titanium white production techniqueThimble joint, is also one of the most key processing step of whole technology controlling and process, and the degree of purity of intermediate product affects titanium dioxide qualityAnd quality.
Metatitanic acid, except mainly for the preparation of titanium dioxide, is also used to prepare Nano titanium dioxide, titanium sulfate, sulphurAcid oxygen titaniums etc. are containing titanium products. Because of raw material place of production difference, preparation technology's difference and add the impact of each factors such as raw material, systemMetatitanic acid in can contain a large amount of impurity metal ions such as iron, cobalt, chromium, magnesium, manganese, alum, niobium, sodium or potassium that comprise, these are assortedThe existence of matter is the greatest factor that affects metatitanic acid quality and quality, and the titanium dioxide form and aspect that calcining obtains are partially yellow, partially red, make itWhiteness is impaired; While preparing Nano titanium dioxide with the metatitanic acid that contains metal impurities, wherein impurity can become nucleus of crystal, makesNano titanium dioxide particle knot is poly-, causes size distribution to be inhomogeneous state, and then has influence on the effect of its catalytic applications; ?In the preparation technology of titanium sulfate or titanyl sulfate, the impurity of metatitanic acid can make the crystal formation of product and structure change, Jin EryingRing solubility and the product purity of product, to downstream product, preparation brings sizable trouble.
Therefore, purifying metatitanic acid, especially separates impurity metal ion wherein, is very necessary, but existing pureChange technology is unsatisfactory, and existing purification technique means adopt washing, bleaching, salt to process continuous treatment step and purify inclined to one side titaniumAcid, the technical problem of its existence is to introduce new residual contamination, in bleaching, using maximum is zinc bleaching agent or aluminium bleaching agent,Be in metatitanic acid, introduce that residue pollutes dye one of source; The potash, the phosphoric acid etc. that in salt processing procedure, use, also can beIn end-product, introduce residual impurity, and then affect purity and the quality of subsequent product.
Summary of the invention
The goal of the invention of patent application of the present invention is impurity metal ion in metatitanic acid to separate and can not introduceThe metatitanic acid purification process of realizing the real purification of metatitanic acid of new impurity. The metatitanic acid purification process that patent application of the present invention providesTechnical scheme, its main technical content is: a kind of metatitanic acid purification process, this purification process is: contain impurity metal ionMetatitanic acid successively through pickle pickling, sedimentation and ion-exchange, return to again the continuous-flow cycle for the treatment of process of pickling, describedPickle is that initial concentration is the aqueous sulfuric acid of 0.05 ~ 2wt%, and the primary quantity of pickle is the metatitanic acid that is placed in pickling tank2～50 times of quality, wherein the stirring of pickling will make metatitanic acid dispersed in aqueous sulfuric acid, in described sedimentation, heavyThe metatitanic acid falling backflows to pickling, and supernatant flows and introduces ion-exchange step, carries out ion-exchange in ion exchange column, circulationProcess is not less than 3 hours, and after cyclic process finishes, the metatitanic acid of filter acid cleaning of evaporator lower floor, through routine washing, dehydration, obtains pureChange metatitanic acid; In ion exchange column, be filled with macroporous type or gel-type strongly acidic cation exchange resin, the ionic of this resinFor Hydrogen.
As a preferred version of technique scheme, the concentration of aqueous sulfuric acid is 0.1 ~ 1wt%.
As a preferred version of technique scheme, the addition of aqueous sulfuric acid is 3～20 times of metatitanic acid quality.
As a preferred version of technique scheme, a whole set of continuous circulation time is 3 ~ 30 hours, and best follows continuouslyThe ring time is 5 ~ 15 hours.
As a preferred version of technique scheme, described metatitanic acid be ilmenite through sulfuric acid solution obtain titanium liquid,The metatitanic acid obtaining after hydrolysis again, and this metatitanic acid has passed through preliminary washing.
As a preferred version of technique scheme, described infall process adopts vertical-flow settler or inclined tube-type to sinkDevice falls.
As a preferred version of technique scheme, described aqueous sulfuric acid is industrial sulphuric acid or chemical reagent sulphurThe dilute sulfuric acid of acid and deionized water mixture.
The metatitanic acid purification process technical scheme of Patent Application Publication of the present invention is the purification work of normal temperature, low sulfuric acid concentrationProcess, adopts low-concentration sulfuric acid to carry out pickling to the metatitanic acid that contains impurity metal ion, and sulfuric acid infiltrates into metatitanic acid particleIn, react with metal ion generate soluble sulphate, as ferrous sulfate, chromium sulfate, vanadic sulfate etc., these soluble-salts withSupernatant is introduced in ion exchange column, with ion exchange resin generation displacement reaction, resin effectively catching metal sun wherein fromSon, sulfate ion is combined with the hydrogen ion of resin and is formed new sulfuric acid, and in a whole set of cyclic process, the sulfuric acid of pickle is denseDegree can remain unchanged at initial level all the time, and the acid sulfate producing that also makes is not hydrolyzed, do not form precipitation, byIon exchange resin is held back and is effectively separated. Another large advantage of the technical program is: fresh sulfuric acid constantly returnsReturn pickling tank, the sulfate being adsorbed in metatitanic acid is had to good leaching effect, thus can be by this part sulfate impuritiesEffectively peel off out, make it depart from metatitanic acid, enter in solution, further improved purifying, removal of impurities effect to metatitanic acid.The purifying metatitanic acid finally obtaining through the process of this programme, can be directly used in calcining, make high-quality titanium dioxide, and withoutAgain through bleaching and salt processing, thereby do not have new impurity and be introduced into. The technical program technique is simple, be easy to realize, pickleSubstantially do not consume, energy consumption is low, water consumption is few, and the product purification quality obtaining is high, low-concentration sulfuric acid pickle wherein canUnrestrictedly recycle. Final purifying metatitanic acid can be for the preparation of high-quality titanium dioxide, Nano titanium dioxide, sulfuric acidThe downstream product such as titanium, titanyl sulfate.
Detailed description of the invention
Embodiment 1
Its processing step, hands over 500ml there-necked flask, glass settler, circulating pump and 100ml ion as pickling tankChange post emulsion tube and be connected to closed circuit, wherein on there-necked flask, assemble 40W stirring motor, in ion exchange column, fill 60mlHydrogen D001 macropore strong acid cation exchanger resin. In above-mentioned closed circuit, add 1wt% aqueous sulfuric acid 300g, three mouthfulsIn flask, dose the metatitanic acid 100g of preliminary washing, start stirring motor and make metatitanic acid dispersed, ON cycle pump, drives thereafterMoving pickle circulates. Continuous circulation operation, after 5 hours, is closed agitator and circulating pump, by emitting inclined to one side titanium in there-necked flaskAcid and water, after filtration, clean, dehydration obtains metatitanic acid after purifying. What table 1 showed is without the preliminary washing metatitanic acid sample purifyingThe impurity content that product and the present embodiment purification process obtain metatitanic acid sample detects contrast table:
Table 1(unit: %)
| Sample \ project | TiO2 | Moisture | Fe2O3 | Cr | V | Al | Mn | Mg |
| Metatitanic acid | 35 | 62 | 0.009 | 0.005 | 0.006 | 0.01 | 0.0001 | 0.002 |
| Essence metatitanic acid | 37 | 61 | 0.0008 | 0.001 | 0.001 | 0.008 | 0.00001 | 0.0004 |
What table 2 showed is metatitanic acid sample and the present embodiment purifying that adopts existing bleaching, salt treatment and purification technique to obtainThe impurity content that method obtains metatitanic acid sample detects contrast table:
Table 2(unit: %)
| Sample \ project | Fe2O3 | Cr | V | Al | K |
| Through the metatitanic acid of bleaching, salt processing | 0.002 | 0.003 | 0.003 | 0.03 | 0.002 |
| Essence metatitanic acid | 0.0008 | 0.001 | 0.001 | 0.008 | 0.00001 |
The existing process for purifying adopting also adopts the metatitanic acid of same preliminary washing, uses titanium dioxide industry traditionalAluminium powder bleaching and potash salt processing method, concrete operations are as follows:
Step 1: acid-soluble
The there-necked flask of being furnished with agitating device is placed on water-bath, adds the metatitanic acid of the preliminary washing of 200g, adds water800ml, adds people 98% industrial sulphuric acid 60g under stirring thereafter, is warming up to 70 ~ 75 DEG C, keeps 1 hour;
Step 2: bleaching reduction
In there-necked flask, add people 1g aluminium powder, after stirring, continue heating, in 80 ~ 90 DEG C, be incubated 2 hours, thenBe cooled to below 45 DEG C, filter out acid solution;
Step 3: washing
Be washed to pH=3 by deionized water, and in there-necked flask, retain a part of water;
Step 4: salt processing
In there-necked flask, first add people 0.8g potash, stirring after 1 hour, then to add 0.2g concentration be 85% phosphoric acid, continueContinuous stirring 1 hour, is washed to neutrality, and the moisture in filtering metatitanic acid obtains the metatitanic acid sample through bleaching and salt processing.
Table 2 correction data shows, compared with existing purification techniques, the purification process of the present patent application makes metatitanic acid impurityContent obviously reduces, with the obvious advantage compared with traditional bleaching, salt treatment and purification method.
Embodiment 2
Add to the closed circuit being connected by emulsion tube with ion exchange column by there-necked flask, glass settler, circulating pumpConcentration is the aqueous sulfuric acid 300g of 1wt%, in there-necked flask, doses metatitanic acid 15g, starts stirring motor and makes metatitanic acid evenAfter dispersion, start circulating pump and start purification cycle work, after 15 hours, stop stirring, closing circulating pump, filtered by there-necked flaskGo out metatitanic acid, obtain purifying metatitanic acid through cleaning, dewatering. Purifying metatitanic acid sample carries out respectively impurity with initial metatitanic acid sampleContent detection, its correction data is as shown in table 3:
Table 3(unit: %)
| Sample \ project | TiO2 | Moisture | Fe2O3 | Cr | V | Al | Mn | Mg |
| Metatitanic acid | 35 | 62 | 0.009 | 0.005 | 0.006 | 0.01 | 0.0001 | 0.002 |
| Essence metatitanic acid | 38 | 60 | 0.0005 | 0.0006 | 0.0005 | 0.004 | 0.00001 | 0.0003 |
Embodiment 3
With pipeline by 2000 liters of enamel still, inclined tube settler, centrifugal pump and 1m that are furnished with agitating device3Ion exchange column is complied withFig. 1 is connected to closed circuit, is filled with 600kg Hydrogen gel type cation exchanger resin in ion exchange column. Described circulationThe sulfuric acid 2000kg that drops into 0.1wt% in loop, doses metatitanic acid 100kg in enamel still, start stirring motor, makes metatitanic acid equalAfter even dispersion, ON cycle pump makes sulfuric acid circulation with the flow of 5000L/hr, after 15 hours, stops stirring, closing circulating pump, byIn enamel still, take out metatitanic acid, after washing, dehydration, obtain purifying metatitanic acid, purifying metatitanic acid sample and initial metatitanic acid sampleCarry out respectively impurity content detection, its correction data is as shown in table 4:
Table 4(unit: %)
| Sample \ project | TiO2 | Moisture | Fe2O3 | Cr | V | Al | Mn | Mg |
| Metatitanic acid | 38 | 60 | 0.015 | 0.009 | 0.009 | 0.015 | 0.001 | 0.002 |
| Essence metatitanic acid | 37 | 61 | 0.0006 | 0.0008 | 0.0008 | 0.005 | 0.00003 | 0.0004 |
Claims (7)
1. a metatitanic acid purification process, is characterized in that this purification process is: the metatitanic acid that contains impurity metal ion successivelyThrough pickle pickling, sedimentation and ion-exchange, return to again the continuous-flow cycle for the treatment of process of pickling, at the beginning of described pickle isBeginning concentration is the aqueous sulfuric acid of 0.05 ~ 2wt%, the primary quantity of pickle be placed in pickling tank metatitanic acid quality 2～50Doubly, wherein the stirring of pickling will make metatitanic acid dispersed in aqueous sulfuric acid, and in described sedimentation, the metatitanic acid of sedimentation returnsFlow to pickling, supernatant flows and introduces ion-exchange step, carries out ion-exchange in ion exchange column, and cyclic process is not less than 3Hour, after cyclic process finishes, the metatitanic acid of filter acid cleaning of evaporator lower floor, through routine washing, dehydration, obtains purifying metatitanic acid; FromIn sub-exchange column, be filled with macroporous type or gel-type strongly acidic cation exchange resin, the ionic of this resin is Hydrogen.
2. metatitanic acid purification process according to claim 1, the concentration that it is characterized in that aqueous sulfuric acid is 0.1 ~ 1wt%.
3. metatitanic acid purification process according to claim 1, the addition that it is characterized in that aqueous sulfuric acid is metatitanic acid3～20 times of quality.
4. metatitanic acid purification process according to claim 1, is characterized in that a whole set of continuous circulation time is 3 ~ 30 hours.
5. metatitanic acid purification process according to claim 4, is characterized in that a whole set of continuous circulation time is 5 ~ 15 hours.
6. metatitanic acid purification process according to claim 1, is characterized in that described metatitanic acid is that ilmenite is through sulfuric acidAcidolysis obtains titanium liquid, the metatitanic acid that obtains after hydrolysis again, and this metatitanic acid has passed through preliminary washing.
7. metatitanic acid purification process according to claim 1, it is characterized in that described aqueous sulfuric acid be industrial sulphuric acid,Or the dilute sulfuric acid of chemical reagent sulfuric acid and deionized water mixture.
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| CN105858721A (en) * | 2016-03-31 | 2016-08-17 | 无锡治洁超材料科技有限公司 | Preparation method of monoatomic layer titanium oxide nanosheet colloidal solution |
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