CN104743606A - Metatitanic acid purifying method - Google Patents
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- CN104743606A CN104743606A CN201510103846.2A CN201510103846A CN104743606A CN 104743606 A CN104743606 A CN 104743606A CN 201510103846 A CN201510103846 A CN 201510103846A CN 104743606 A CN104743606 A CN 104743606A
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- metatitanic acid
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- 239000002253 acid Substances 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000005342 ion exchange Methods 0.000 claims abstract description 20
- 238000005554 pickling Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 59
- 238000000746 purification Methods 0.000 claims description 23
- 235000021110 pickles Nutrition 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 6
- 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 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 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
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 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 21
- 239000004408 titanium dioxide Substances 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 6
- 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 4
- 229910000349 titanium oxysulfate Inorganic materials 0.000 abstract description 4
- 229910000348 titanium sulfate Inorganic materials 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005112 continuous flow technique Methods 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- 235000010215 titanium dioxide Nutrition 0.000 description 10
- 238000004061 bleaching Methods 0.000 description 9
- 241000218218 Ficus <angiosperm> Species 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 238000001514 detection method Methods 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
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 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
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 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
- 238000001556 precipitation Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011701 zinc Substances 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
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical class [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 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
- 238000009826 distribution Methods 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 239000012467 final product 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
- 238000007654 immersion Methods 0.000 description 1
- 230000001771 impaired effect Effects 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
- 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
- 150000001457 metallic cations Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 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
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Abstract
The invention provides a metatitanic acid purifying method. The metatitanic acid purifying method is characterized in that a pickling solution is subjected to a continuous flow processing and circulating process namely pickling, settling, ion exchanging and pickling in sequence, wherein metatitanic acid in settling refluxes to be subjected to pickling; liquid supernatant flows to be introduced into an ion exchange step to perform ion exchange in an ion exchange column, and the circulating process is not less than three hours; after the circulating process is ended, metatitanic acid at the lower layer of the pickling tank is filtered, and then is subjected to normal washing and dehydrating to obtain the purified metatitanic acid. According to the technical scheme adopted by the invention, the process is simple and easy to realize, the picking solution is almost not consumed, the energy consumption is low, the water consumption is low, and the final purified metatitanic acid can be used for preparing downstream products of high-quality titanium dioxide, nano titanium dioxide, titanium sulfate, titanyl sulfate and the like.
Description
Technical field
Patent application of the present invention relates to metatitanic acid purifying method, is in particular separated from metatitanic acid by metallic impurity, makes metatitanic acid be able to pure processing method.
Background technology
Metatitanic acid is the intermediate product of a core procedure in titanium dioxide manufacturing process.The predominant methods preparing titanium dioxide is sulfuric acid process, and the method take ilmenite as raw material, and obtain titanium liquid through sulfuric acid solution, titanium liquid is again through being hydrolyzed obtained hydrated titanium dioxide, i.e. intermediate product metatitanic acid, metatitanic acid obtains titanium dioxide through high-temperature calcination again.The preparation of metatitanic acid is the core link of titanium white production technique, and be also one of the most key processing step of whole technology controlling and process, the purity of intermediate product affects titanium dioxide quality and quality.
Metatitanic acid, except mainly for the preparation of except titanium dioxide, is also used to prepare Nano titanium dioxide, titanium sulfate, titanyl sulfate etc. containing titanium products.Because the starting material place of production is different, the difference of preparation technology and add the impact of each factors such as raw material, the impurity metal ions such as iron, cobalt, chromium, magnesium, manganese, alum, niobium, sodium or potassium can be comprised containing a large amount of in obtained metatitanic acid, the existence of these impurity is the most important factor affecting metatitanic acid quality and quality, calcine the titanium dioxide form and aspect obtained partially yellow, partially red, make its whiteness impaired; When preparing Nano titanium dioxide with the metatitanic acid containing metallic impurity, wherein impurity can become nucleus of crystal, Nano titanium dioxide particle is tied poly-, causes size-grade distribution to be uneven state, and then have 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, and then affects solubleness and the product purity of product, brings sizable trouble to derived product preparation.
Therefore, purifying metatitanic acid, especially impurity metal ion is wherein separated, very necessary, but existing purification technique is unsatisfactory, existing purification technique means adopt washing, bleaching, the continuous treatment step of Ficus caricaL to purify metatitanic acid, and its technical problem existed to introduce new residual contamination, using maximum in bleaching is zinc SYNTHETIC OPTICAL WHITNER or aluminium SYNTHETIC OPTICAL WHITNER, is in metatitanic acid, introduce one of dye source that residue pollutes; The salt of wormwood used in Ficus caricaL process, phosphoric acid etc., also can introduce residual impurity, and then affect purity and the quality of subsequent product in final product.
Summary of the invention
The goal of the invention of patent application of the present invention be impurity metal ion in metatitanic acid to separate and can not introduce new impurity realize the metatitanic acid purification process that metatitanic acid really purifies.The metatitanic acid purification process technical scheme that patent application of the present invention provides, its main technical content is: a kind of metatitanic acid purification process, for pickle solution is successively through pickling, sedimentation and ion-exchange, return the continuous flow cycle for the treatment of process of pickling again, the aqueous sulfuric acid of described pickle solution to be starting point concentration be 0.05 ~ 2wt%, the original bulk of pickle solution is 2 ~ 50 times of the metatitanic acid quality being placed in pickling tank, wherein the stirring of pickling will make metatitanic acid dispersed in aqueous sulfuric acid, in described sedimentation, the metatitanic acid of sedimentation backflows to pickling, ion-exchange step is introduced in supernatant liquor flowing, ion-exchange is carried out in ion exchange column, working cycle is not less than 3 hours, after working cycle terminates, the metatitanic acid of filter acid cleaning of evaporator lower floor, through conventional water wash, dehydration, obtain purifying metatitanic acid, be filled with macroporous type or gel-type strongly acidic cation exchange resin in ion exchange column, the ionic of this resin is 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 add-on 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 the best continuous circulation time is 5 ~ 15 hours.
As a preferred version of technique scheme, described metatitanic acid is the metatitanic acid that ilmenite obtains titanium liquid through sulfuric acid solution, obtains after hydrolysis, and this metatitanic acid have passed through preliminary washing.
As a preferred version of technique scheme, described settling process adopts vertical-flow settling vessel or inclined tube-type settling vessel.
As a preferred version of technique scheme, described aqueous sulfuric acid is the dilute sulphuric acid of industrial sulphuric acid or chemical reagent sulfuric acid and deionized water mixture.
Metatitanic acid purification process technical scheme disclosed in patent application of the present invention, for normal temperature, the technological process for purifying of low sulfuric acid concentration, low-concentration sulfuric acid is adopted to carry out pickling to the metatitanic acid containing impurity metal ion, sulfuric acid infiltrates in metatitanic acid particle, react with metal ion and generate soluble sulphate, as ferrous sulfate, chromium sulphate, vanadylic sulfate etc., these soluble salts are introduced in ion exchange column with supernatant liquor, with ion exchange resin generation replacement(metathesis)reaction, resin effectively catching metallic cation wherein, sulfate ion is then combined with the hydrogen ion of resin and forms new sulfuric acid, namely in a whole set of working cycle, the sulfuric acid concentration of pickle solution can remain unchanged at initial level all the time, and acidity also makes the vitriol of generation not be hydrolyzed, do not form precipitation, retained by ion exchange resin and effectively separated.Another large advantage of the technical program is: fresh sulfuric acid constantly returns pickling tank, good immersion Zn is had to the vitriol be adsorbed in metatitanic acid, thus this part sulfate impurities effectively can be stripped out, it is made to depart from metatitanic acid, enter in solution, further increase the purifying to metatitanic acid, removal of impurities effect.Through the purifying metatitanic acid that the processing method of this programme finally obtains, calcining, obtained high-quality titanium dioxide can be directly used in, and without the need to again through bleaching and Ficus caricaL, thus not have new impurity and be introduced into.The technical program technique is simple, be easy to realize, pickle solution does not consume substantially, energy consumption is low, water consumption is few, and the product purification quality obtained is high, and low-concentration sulfuric acid pickle solution wherein can unrestrictedly recycle.Final purifying metatitanic acid may be used for preparing the derived product such as high-quality titanium dioxide, Nano titanium dioxide, titanium sulfate, titanyl sulfate.
Embodiment
embodiment 1
Its processing step is, using as pickling tank 500ml there-necked flask, glass settling vessel, recycle pump is connected with emulsion tube with 100ml ion exchange column is circulation loop, wherein there-necked flask assembles 40W agitator motor, in ion exchange column, fill 60ml Hydrogen D001 macropore strong acid cation exchange resin.In above-mentioned circulation loop, add 1wt% aqueous sulfuric acid 300g, in there-necked flask, dose the metatitanic acid 100g of initial water wash, start agitator motor and make metatitanic acid dispersed, ON cycle pump thereafter, drive pickle solution to circulate.After continuous circulation runs 5 hours, close agitator and recycle pump, by releasing metatitanic acid and water in there-necked flask, after filtration, cleaning, dehydration obtain metatitanic acid after purifying.What table 1 showed is the foreign matter content detection contrast table obtaining metatitanic acid sample without the initial water wash metatitanic acid sample purified and the present embodiment purification process:
Table 1 (unit: %)
| Sample \ project | TiO 2 | Moisture | Fe 2O 3 | 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 |
The foreign matter content that the metatitanic acid sample that what table 2 showed is adopts existing bleaching, Ficus caricaL purification process obtains and the present embodiment purification process obtain metatitanic acid sample detects contrast table:
Table 2 (unit: %)
| Sample \ project | Fe 2O 3 | Cr | V | Al | K |
| Through the metatitanic acid of bleaching, Ficus caricaL | 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 purification process adopted also adopts the metatitanic acid of same initial water wash, the aluminium powder bleaching using titanium dioxide industry traditional and potash salt treatment process, and concrete operations are as follows:
Step 1: acid-soluble
The there-necked flask being furnished with whipping appts is placed on water-bath, adds the metatitanic acid of 200g initial water wash, and add water 800ml, adds the industrial sulphuric acid 60g of people 98%, be warming up to 70 ~ 75 DEG C, keep 1 hour under stirring thereafter;
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, be then cooled to less than 45 DEG C, filter out acidic solution;
Step 3: washing
Be washed to pH=3 with deionized water, and in there-necked flask, retain a part of water;
Step 4: Ficus caricaL
In there-necked flask, first add people 0.8g salt of wormwood, after one hour of the stirring, then to add 0.2g concentration be 85% phosphoric acid, continues stirring 1 hour, be washed to neutrality, the moisture in filtering metatitanic acid, obtains the metatitanic acid sample through bleaching and Ficus caricaL.
Table 2 correlation data shows, compared with existing purification techniques, the purification process of the present patent application makes metatitanic acid foreign matter content obviously reduce, with the obvious advantage compared with traditional bleaching, Ficus caricaL purifying method.
embodiment 2
The aqueous sulfuric acid 300g that concentration is 1wt% is added to the circulation loop be connected by emulsion tube by there-necked flask, glass settling vessel, recycle pump and ion exchange column, metatitanic acid 15g is dosed in there-necked flask, after startup agitator motor makes metatitanic acid dispersed, start recycle pump and start purification cycle work, after 15 hours, stop stirring, closing recycle pump, filter out metatitanic acid by there-necked flask, obtain purifying metatitanic acid through cleaning, dehydration.Purifying metatitanic acid sample and initial metatitanic acid sample carry out foreign matter content detection respectively, and its correlation data is as shown in table 3:
Table 3 (unit: %)
| Sample \ project | TiO 2 | Moisture | Fe 2O 3 | 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
2000 liters be furnished with the enamel still of whipping appts, inclined tube settler, impeller pump and 1m with pipeline
3ion exchange column connects for circulation loop, is filled with 600kg Hydrogen gel-network precipitation method in ion exchange column.The sulfuric acid 2000kg of 0.1wt% is dropped in described circulation loop, metatitanic acid 100kg is dosed in enamel still, start agitator motor, after making metatitanic acid dispersed, ON cycle pump makes sulfuric acid circulate with the flow of 5000L/hr, after 15 hours, stop stirring, closing recycle pump, take out metatitanic acid by enamel still, after washing, dehydration, obtain purifying metatitanic acid, purifying metatitanic acid sample and initial metatitanic acid sample carry out foreign matter content detection respectively, and its correlation data is as shown in table 4:
Table 4 (unit: %)
| Sample \ project | TiO 2 | Moisture | Fe 2O 3 | 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, it is characterized in that this purification process is that pickle solution is successively through pickling, sedimentation and ion-exchange, return the continuous flow cycle for the treatment of process of pickling again, the aqueous sulfuric acid of described pickle solution to be starting point concentration be 0.05 ~ 2wt%, the original bulk of pickle solution is 2 ~ 50 times of the metatitanic acid quality being placed in pickling tank, wherein the stirring of pickling will make metatitanic acid dispersed in aqueous sulfuric acid, in described sedimentation, the metatitanic acid of sedimentation backflows to pickling, ion-exchange step is introduced in supernatant liquor flowing, ion-exchange is carried out in ion exchange column, working cycle is not less than 3 hours, after working cycle terminates, the metatitanic acid of filter acid cleaning of evaporator lower floor, through conventional water wash, dehydration, obtain purifying metatitanic acid, be filled with macroporous type or gel-type strongly acidic cation exchange resin in ion exchange column, the ionic of this resin is Hydrogen.
2. metatitanic acid purification process according to claim 1, is characterized in that the concentration of aqueous sulfuric acid is 0.1 ~ 1wt%.
3. metatitanic acid purification process according to claim 1, is characterized in that the add-on of aqueous sulfuric acid is 3 ~ 20 times of metatitanic acid 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, it is characterized in that described metatitanic acid is the metatitanic acid that ilmenite obtains titanium liquid through sulfuric acid solution, obtains after hydrolysis, and this metatitanic acid have passed through preliminary washing.
7. metatitanic acid purification process according to claim 1, is characterized in that described aqueous sulfuric acid is the dilute sulphuric acid of industrial sulphuric acid or chemical reagent sulfuric acid and deionized water mixture.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN108993618A (en) * | 2018-08-28 | 2018-12-14 | 梧州黄埔化工药业有限公司 | A kind of regeneration technology of synthetic borneol metatitanic acid catalyst |
| CN109467121A (en) * | 2018-12-26 | 2019-03-15 | 江苏中研创星材料科技有限公司 | The method of the removal of impurities of metatitanic acid |
| CN109534392A (en) * | 2018-12-27 | 2019-03-29 | 中钛集团焦作市裕盛钛业有限公司 | A kind of production technology of food-level titanium dioxide |
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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 |
| CN108993618A (en) * | 2018-08-28 | 2018-12-14 | 梧州黄埔化工药业有限公司 | A kind of regeneration technology of synthetic borneol metatitanic acid catalyst |
| CN109467121A (en) * | 2018-12-26 | 2019-03-15 | 江苏中研创星材料科技有限公司 | The method of the removal of impurities of metatitanic acid |
| CN109534392A (en) * | 2018-12-27 | 2019-03-29 | 中钛集团焦作市裕盛钛业有限公司 | A kind of production technology of food-level titanium dioxide |
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| CN104743606B (en) | 2016-05-18 |
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