CN104071835B - A kind of preparation method of titanium dioxide - Google Patents
A kind of preparation method of titanium dioxide Download PDFInfo
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- CN104071835B CN104071835B CN201410305431.9A CN201410305431A CN104071835B CN 104071835 B CN104071835 B CN 104071835B CN 201410305431 A CN201410305431 A CN 201410305431A CN 104071835 B CN104071835 B CN 104071835B
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Abstract
The invention discloses a kind of preparation method of titanium dioxide, the method comprises: titaniferous material is carried out successively acidolysis process, leaching process, reduction treatment, settlement treatment, hydrolysis treatment and calcination processing, wherein, in described acidolysis process and leaching process, in reaction system, pressurized air is passed into, after leaching process terminates, stop passing into described pressurized air, and under agitation, the material after leaching process and reductive agent are carried out contact reacts, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.06-0.95).Adopt method of the present invention can reduce the consumption of reductive agent, and obtain the higher titanium dioxide of whiteness.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide.
Background technology
In the technique of Titanium White Production By Sulfuric Acid Process (titanium dioxide), because ferric hydrolysis pH and titanium hydrolysis pH is close, if there is ferric ion in titanium liquid, so will produce more ferric hydrolysate be adsorbed onto titanium dioxide surface and be difficult to rinse well in the titanium hydrolysis process of production technique, affect the whiteness of the titanium dioxide product of final production.Usually, in order to prevent the ferrous ions in the titanium liquid after acidolysis from becoming ferric ion, just requiring containing finite concentration trivalent titanium ion in titanium liquid, thus iron in each process procedure subsequently can be kept to exist with the form of ferrous ion.Traditional method partial-titanium in titanium liquid being reduced to titanous adds iron powder in the titanium liquid after directly completing to acidolysis in acidolysis device under passing into compressed-air actuated condition, and carry out reduction reaction at about 70 DEG C.But producing titanium dioxide by the method needs to use a large amount of iron powders, there is the problem that preparation cost is high.
Summary of the invention
The object of the invention is to overcome the problem that in existing Titanium White Production By Sulfuric Acid Process technique, iron powder consumption is large, cost is high, provide the preparation method of the titanium dioxide that a kind of reductive agent consumption is little, cost is low.
The present inventor finds through further investigation, in the process preparing titanium dioxide, if passing under pressurized air stirs, in acidolysis device, directly carry out iron powder reducing process can cause the consumption of iron powder larger, in order to overcome this defect, contriver stopped compressed-air actuated passing into after leaching process terminates, and in reduction treatment, adopt other alr modes except passing into pressurized air, thus overcome above-mentioned defect, reduce the consumption of reductive agent, thus complete the present invention.
In addition, the present inventor infers that the reason that can reduce the consumption of reductive agent is: in the present invention, after leaching process terminates, stop passing into described pressurized air, the titanous restored in reduction reaction can be prevented thus to be reoxidized into titanic and ferric iron with ferrous iron, thus be again reduced into titanous and ferrous iron without the need to the titanic that again this is again oxidized to by reductive agent and ferric iron, significantly reduce the consumption of reductive agent thus.
To achieve these goals, the invention provides a kind of preparation method of titanium dioxide, the method comprises: titaniferous material is carried out successively acidolysis process, leaching process, reduction treatment, settlement treatment, hydrolysis treatment and calcination processing, wherein, in described acidolysis process and leaching process, in reaction system, pass into pressurized air, after leaching process terminates, stop passing into described pressurized air, and under agitation, material after leaching process and reductive agent are carried out contact reacts, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.06-0.95).
By adopting the preparation method of titanium dioxide of the present invention, owing to stopped compressed-air actuated passing into after leaching process terminates, the titanium leaching liquid that can meet the demands with the reductive agent of lower consumption acquisition titanous concentration thus, thus obtain the higher titanium dioxide of whiteness, reduce into product cost, increase production efficiency.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of titanium dioxide, the method comprises: titaniferous material is carried out successively acidolysis process, leaching process, reduction treatment, settlement treatment, hydrolysis treatment and calcination processing, wherein, in described acidolysis process and leaching process, in reaction system, pressurized air is passed into, after leaching process terminates, stop passing into described pressurized air, and under agitation, the material after leaching process and reductive agent are carried out contact reacts, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.06-0.95).
The present inventor also finds, because the material after acidolysis can solidify in maturing process, in acidolysis device, directly install whipping appts is inappropriate for suitability for industrialized production, therefore, particularly preferably, contriver is sent in outside reducing bath by acidolysis device through the material of leaching process, and reduction treatment is carried out under mechanical stirring in this reducing bath, thus both successfully avoided the defect that adopts pressurized air to stir in existing reduction treatment thus reduced the consumption of iron powder or iron filings, the industrial production of serialization can be realized again.What deserves to be explained is, in the present invention, although passing into compressed-air actuated object is also to stir, in reduction treatment, described agitation condition does not comprise this and passes into compressed-air actuated alr mode, and it can be mechanical stirring, magnetic agitation or ultrasonic stirring.
One of the present invention preferred embodiment in, the preparation method of described titanium dioxide comprises: titaniferous material is carried out successively acidolysis process, leaching process, reduction treatment, settlement treatment, hydrolysis treatment and calcination processing, wherein, described acidolysis process and leaching process carry out in acidolysis device, and after leaching process terminates, stop passing into described pressurized air, and the material after leaching process is sent in reducing bath, under mechanical agitation, material after leaching process and reductive agent are carried out contact reacts, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.06-0.95).Here reducing bath is the outside independent of acidolysis device, and it is configured with mechanical stirring device.Adopt this preferred embodiment, not only can realize, to the reduction of described reductive agent consumption, the continuous industrial production of titanium dioxide can also being realized, low cost high yield.
The titanium material that common method for producing gtitanium dioxide with sulphuric acid adopts is selected ilmenite and ilmenite concentrate that titanium content is higher and is smelted the titanium slag etc. obtained by ilmenite concentrate.Owing to having eliminated most of iron in titanium slag smelting process and having contained more titanous, the titanium liquid thus after titanium slag acidolysis has not needed to reduce.Therefore, in the present invention, described titaniferous material is particularly preferably ilmenite etc. without the titaniferous ore smelted.In addition, the titanium content of described titaniferous material is (with TiO
2meter) be preferably 40-60 % by weight.
According to the present invention, described titaniferous material is for the ease of acidolysis process, screen over-size below preferred employing 325 order is the titaniferous material (cross 325 object sieves by titaniferous material, the coarse grained amount of not sifting out is only less than 15 % by weight of the total amount of titaniferous material) of less than 15 % by weight.
According to the present invention, described acidolysis process can adopt conventional acid system to prepare acidolysis treatment process in the technique of titanium dioxide, such as, sulphuric acid soln in system is diluted to 84-86 % by weight by the sulphuric acid soln or the water that add about 20-25 % by weight after being mixed with the sulphuric acid soln of about 90-94 % by weight by titaniferous material, in dilution, temperature of reaction system can be raised to about 80-120 DEG C by liberated heat, and the iron at this temperature in titanium ore, magnesium, calcium etc. are in succession continuous mutually with sulfuric acid reaction releases heat temperature is raised to about 150-180 DEG C.The consumption of sulphuric acid soln can adjust according to the amount of titaniferous material and composition, and such as, the titanium of the 40-60 % by weight relative to 1 ton is (with TiO
2meter) ilmenite concentrate, the amount of the sulphuric acid soln of the 84-86 % by weight in system can be 1450-1650kg.In addition, the solvent of sulphuric acid soln is preferably water.
Usually, in described acidolysis process, in order to make sulphuric acid soln and titaniferous material reaction more fully, can pass into pressurized air and stirring, such as employing passes into speed and is preferably 1000-1500m
3the pressurized air of/h; until acidolysis reaction terminates; and the acid hydrolysate (such as titanyl sulfate) in order to obtain more titanium; usually the material after by acidolysis is also needed preferably to carry out insulation slaking; need to add water or dilute sulphuric acid after insulation slaking the acid hydrolysate solidified in slaking dilution is leached namely to carry out described leaching and process, in described leaching treating processes, also need to pass into pressurized air (pass into speed and be preferably 200-400m
3/ h) stir, in leaching material out, the content of titanium elements is (with TiO
2meter) be preferably 120-140g/L, and carry other lysate and insoluble small particles material simultaneously.And acidolysis process of the present invention and leaching process also can adopt such method to carry out.
But contain ferric ion merely through in the material after acidolysis process and leaching process, in reduction treatment, main purpose is just ferric ion to be reduced to ferrous ion, produce a certain amount of trivalent titanium ion simultaneously, the titanous particle produced can ensure that ferrous ion is no longer oxidized to ferric ion in other follow-up process, usually, after reduction treatment, need the content of the titanous produced at more than 0.8g/L.And in the present invention, preferably, in the material after the contact reacts in described reduction treatment, the content of titanous is 0.8-2g/L.
According to the present invention, in described reduction treatment, described reductive agent can be that this area routine is preparing titanium dioxide such as, for reducing ferric iron and titanic reductive agent, iron filings and/or iron powder, is preferably iron powder, is particularly preferably 80-200 object iron powder.
According to the present invention, to be describedly preferably under mechanical agitation under agitation, thus advantageously to avoid the large defect of the reductive agent consumption that produced by dioxygen oxidation in pressurized air whipping process.Under preferable case, with TiO
2meter, titanium elements contained in the material of described acidolysis process and the mol ratio of described reductive agent are 1:(0.07-0.09).
According to the present invention, under preferable case, described reductive agent can add in two batches, wherein, first reductive agent adds before described contact reacts, second batch reductive agent adds after described contact reacts carries out 30min, carries out adding second batch reductive agent between 30-100min particularly preferably in described contact reacts.Under preferable case, be 100 % by weight in total consumption of described reductive agent, first reductive agent described accounts for 80-95 % by weight, and described second batch reductive agent accounts for 5-20 % by weight.
According to the present invention, under preferable case, the condition of described reduction treatment comprises: temperature of reaction is 55-75 DEG C, and the reaction times is 80-130min.More preferably, the condition of described reduction treatment comprises: temperature of reaction is 60-70 DEG C, and the reaction times is 80-100min.
In the preferred embodiment of the present invention, what adopt in reduction treatment is mechanical stirring, and mechanical stirring speed is preferably 10-30rpm/min.
According to the present invention, by titaniferous material after above-mentioned acidolysis process, leaching process and reduction treatment, then the product of titanium dioxide just can be obtained through settlement treatment, hydrolysis treatment and calcination processing.In the present invention, above-mentioned settlement treatment, hydrolysis treatment and calcination processing are not limited especially, as long as the titanium in the leach liquor of the leach liquor of the titaniferous obtained by method of the present invention and titaniferous can be extracted respectively.
Wherein, described settlement treatment can adopt the acid system of this area routine to prepare sedimentation method in titanium dioxide technique, such as described settlement treatment can be add certain proportion flocculation agent to leave standstill in subsider, allow solid particulate flocculating settling in titanium liquid bottom settling bowl, its supernatant liquor is used for hydrolysis treatment.
Wherein, described hydrolysis treatment can adopt the acid system of this area routine to prepare method for hydrolysis in titanium dioxide technique, such as described hydrolysis treatment be by settlement treatment after the process that is hydrolyzed of supernatant liquor, the mode that automatic growing crystal species can be adopted to be hydrolyzed also can be the mode of plus seed hydrolysis.
Wherein, described calcination processing can adopt the acid system of this area routine to prepare method for calcinating in titanium dioxide technique, such as the product (metatitanic acid) after hydrolysis is sent in rotary kiln, mix and calcine with one or more in zinc salt (such as zinc oxide, zinc sulfate, zinc chloride etc.), microcosmic salt (such as phosphoric acid) and sylvite (such as potassium hydroxide, salt of wormwood etc.), to obtain titanium dioxide.
Below will be described the present invention by embodiment.
In following examples and comparative example, the content of titanous is that to adopt with potassium sulfocyanate be indicator, measures by the method for ferric ammonium sulfate standardized solution titration; (b value represents the scope from gold-tinted to blue light to adopt color difference meter to detect titanium dioxide sample b value, its codomain is the b value expression yellow of+127 to-128 ,+127, and the b value of-128 represents blue), b value larger expression sample is more yellow, and b value is whiter the closer to 0 value sample; Ilmenite concentrate particle was 325 object sieves, and the coarse grained amount of not sifting out is the titaniferous material of less than 15 % by weight of the total amount of titaniferous material.
Embodiment 1
The present embodiment is for illustration of the preparation method of titanium dioxide of the present invention.
By the ilmenite concentrate particle of 25000kg (with TiO
2meter, titanium content is 46 % by weight) join together in acidolysis pot with sulphuric acid soln (44117kg, concentration is 85 % by weight), in reaction mass, passing into pressurized air, (passing into speed is 1200m
3/ h), and at 160 DEG C of reaction 25min, then (now temperature is 120 DEG C) after slaking 1.5h, adopt 70m
3water carries out dilution and leaches, and the material after leaching is sent in reducing bath (volume sending into the material in reducing bath is 85m
3, and with TiO
2meter, the concentration of titanium is 130g/L).65 DEG C, under 15rpm/min mechanical stirring speed, add the 80 order iron powders of 500kg, and react 100min, but add the iron powder of 80kg again, then react 30min, the content of the titanous in gained titanium liquid is 1.2g/L.Titanium liquid after reduction is carried out settlement treatment, take out supernatant liquor and send into hydrolytic tank, the supernatant liquor that takes a morsel carries out condensing crystal and adds in hydrolytic tank as crystal seed and be hydrolyzed, obtain metatitanic acid and in rotary kiln (top temperature is 850 DEG C), calcine 4h after washing, obtain the titanium dioxide of 9550kg, b value is 2.
Embodiment 2
The present embodiment is for illustration of the preparation method of titanium dioxide of the present invention.
By the ilmenite concentrate particle of 20000kg (with TiO
2meter, titanium content is 52 % by weight) join together in acidolysis pot with sulphuric acid soln (36213kg, concentration is 84 % by weight), in reaction mass, passing into pressurized air, (passing into speed is 1400m
3/ h), and at 180 DEG C of reaction 17min, then (now temperature is 126 DEG C) after slaking 2h, adopt 60m
3water carries out dilution and leaches, and the material after leaching is sent in reducing bath (volume sending into the material in reducing bath is 74m
3, and with TiO
2meter, the concentration of titanium is 135g/L).70 DEG C, under 20rpm/min mechanical stirring speed, add the 100 order iron powders of 550kg, and react 50min, but add the iron powder of 75kg again, then react 30min, the content of the titanous in gained titanium liquid is 1g/L.By the titanium liquid process after reduction, take out supernatant liquor and send into hydrolytic tank, the supernatant liquor that takes a morsel carries out condensing crystal and adds in hydrolytic tank as crystal seed and be hydrolyzed, obtain metatitanic acid and in rotary kiln (top temperature is 950 DEG C), calcine 4.5h after washing, obtain the titanium dioxide of 9120kg, b value is 2.05.
Embodiment 3
The present embodiment is for illustration of the preparation method of titanium dioxide of the present invention.
By the ilmenite concentrate particle of 30000kg (with TiO
2meter, titanium content is 45 % by weight) join together in acidolysis pot with sulphuric acid soln (53000kg, concentration is 85 % by weight), in reaction mass, passing into pressurized air, (speed of passing into is 1300m
3/ h), and at 175 DEG C of reaction 30min, then (now temperature is 100 DEG C) after slaking 1h, adopt 80m
3water carries out dilution and leaches, and the material after leaching is sent in reducing bath (volume sending into the material in reducing bath is 93m
3, and with TiO
2meter, the concentration of titanium is 140g/L).70 DEG C, under 30rpm/min mechanical stirring speed, add the 200 order iron powders of 660kg, and react 50min, but add the iron powder of 70kg again, then react 30min, the content of the titanous in gained titanium liquid is 1.5g/L.By the titanium liquid process after reduction, take out supernatant liquor and send into hydrolytic tank, the supernatant liquor that takes a morsel carries out condensing crystal and adds in hydrolytic tank as crystal seed and be hydrolyzed, obtain metatitanic acid and in rotary kiln (top temperature is 800 DEG C), calcine 5h after washing, obtain the titanium dioxide of 11450kg, b value is 1.95.
Embodiment 4
The present embodiment is for illustration of the preparation method of titanium dioxide of the present invention.
Method according to embodiment 1, difference is, the disposable iron powder adding 580kg in reduction treatment, and the content of the titanous in gained titanium liquid is 1.1g/L.Obtain the titanium dioxide of 9550kg, b value is 2.1.
Comparative example 1
According to the method for embodiment 1, difference is, directly in acidolysis pot, carries out reduction treatment, and after leaching in dilution, continuing to pass into pressurized air, (speed of passing into is 350m
3/ h), the content of the titanous in gained titanium liquid is 0.5g/L, then obtains the titanium dioxide of 9550kg, and its b value is greater than 3.
Comparative example 2
According to the method for embodiment 4, difference is, directly in acidolysis pot, carries out reduction treatment, and after leaching in dilution, continuing to pass into pressurized air, (speed of passing into is 350m
3/ h), add iron powder 800kg, the content of the titanous in gained titanium liquid is 1.2g/L, and (titanium dioxide, its b value is 2.15 then to obtain 8632kg.
Known by the result of comparing embodiment and comparative example, adopt method of the present invention can reduce the consumption of reductive agent, obtain whiteness higher, the titanium dioxide that output is larger.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method of a titanium dioxide, the method comprises: titaniferous material is carried out successively acidolysis process, leaching process, reduction treatment, settlement treatment, hydrolysis treatment and calcination processing, it is characterized in that, in described acidolysis process and leaching process, in reaction system, pass into pressurized air, after leaching process terminates, stop passing into described pressurized air, and under agitation, the material after leaching process and reductive agent are carried out contact reacts, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.06-0.09); Wherein, the condition of described reduction treatment comprises: temperature of reaction is 55-75 DEG C, and the reaction times is 80-130min.
2. method according to claim 1, wherein, with TiO
2meter, in the material after described leaching process, the mol ratio of contained titanium elements and described reductive agent is 1:(0.07-0.09).
3. method according to claim 1, wherein, described reductive agent is iron powder and/or iron filings.
4. method according to claim 3, wherein, described reductive agent is iron powder.
5. method according to claim 1, wherein, the condition of described reduction treatment comprises: temperature of reaction is 60-70 DEG C, and the reaction times is 80-100min.
6. according to the method in claim 1-5 described in any one, wherein, in described reduction treatment, described reductive agent adds in two batches, first reductive agent adds before described contact reacts, and second batch reductive agent adds after described contact reacts carries out 30min.
7. method according to claim 6, wherein, be 100 % by weight in total consumption of described reductive agent, first reductive agent described accounts for 80-95 % by weight, and described second batch reductive agent accounts for 5-20 % by weight.
8. in the material according to the method in claim 1-5 and 7 described in any one, wherein, after described contact reacts, the content of titanous is 0.8-2g/L.
9. according to the method in claim 1-5 and 7 described in any one, wherein, with TiO
2meter, in the material after described leaching process, the content of titanium elements is 120-140g/L.
10. method according to claim 8, wherein, with TiO
2meter, in the material after described leaching process, the content of titanium elements is 120-140g/L.
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| CN105970006A (en) * | 2016-07-07 | 2016-09-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium dioxide through high-iron-oxide titanium concentrate |
| CN106241867A (en) * | 2016-08-30 | 2016-12-21 | 襄阳龙蟒钛业有限公司 | A kind of preparation method of titanium dioxide |
| CN106957067A (en) * | 2017-04-24 | 2017-07-18 | 四川龙蟒钛业股份有限公司 | Reduce the sulfuric acid method titanium pigment acid hydrolysis method of reduced iron powder consumption |
| CN108502920A (en) * | 2018-03-28 | 2018-09-07 | 董小琳 | A kind of preparation process of titanium dioxide |
| CN113122719A (en) * | 2019-12-31 | 2021-07-16 | 中国科学院过程工程研究所 | Method for recovering titanium from red mud leaching solution |
| CN111646502B (en) * | 2020-06-10 | 2022-08-02 | 攀钢集团研究院有限公司 | Slag ore mixing continuous acidolysis leaching method and equipment |
| CN114436323A (en) * | 2021-12-28 | 2022-05-06 | 龙佰襄阳钛业有限公司 | Acidolysis leaching temperature control process |
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| CN103641164A (en) * | 2013-12-09 | 2014-03-19 | 攀钢集团研究院有限公司 | Process for producing titanium dioxide through sulfuric acid method as well as titanyl sulfate solution reduction device and method |
| CN103723765A (en) * | 2014-01-20 | 2014-04-16 | 韶关学院 | Method for preparing titanium dioxide through sulfuric acid method |
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