CN104071835A - Preparation method of titanium dioxide - Google Patents
Preparation method of titanium dioxide Download PDFInfo
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- CN104071835A CN104071835A CN201410305431.9A CN201410305431A CN104071835A CN 104071835 A CN104071835 A CN 104071835A CN 201410305431 A CN201410305431 A CN 201410305431A CN 104071835 A CN104071835 A CN 104071835A
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Abstract
The invention discloses a preparation method of titanium dioxide. The method comprises the following step: sequentially carrying out acidolysis treatment, leaching treatment, reduction treatment, settling treatment, hydrolytic treatment and calcining treatment on a titanium-containing material, wherein the method specially comprises the following steps: in the acidolysis treatment and the leaching treatment, introducing compressed air into a reaction system; after the leaching treatment, stopping introducing the compressed air and carrying out contact reaction on the material after the leaching treatment and a reducing agent under stirring condition, wherein the molar ratio of titanium contained in the material after the leaching treatment and the reducing agent is 1:(0.06-0.95). By adopting the method disclosed by the invention, the use level of the reducing agent can be lowered, and titanium dioxide with high whiteness can be obtained.
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 approach, if there is ferric ion in titanium liquid, in the titanium hydrolysis of production technique is processed, will produce so more ferric hydrolysate and be adsorbed onto titanium dioxide surface and be difficult to and rinse well, affect the whiteness of the titanium dioxide product of final production.Conventionally, in order to prevent that the ferrous ion in the titanium liquid after acidolysis is oxidized to ferric ion, just require to contain in titanium liquid finite concentration trivalent titanium ion, thereby can keep iron in each process procedure subsequently to exist with the form of ferrous ion.The traditional method that partial-titanium in titanium liquid is reduced to titanous is to add iron powder in the titanium liquid passing into after directly completing to acidolysis in acidolysis device under compressed-air actuated condition, and carries out reduction reaction 70 ℃ of left and right.But, by the method, produce titanium dioxide and need 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, the preparation method of the titanium dioxide that a kind of reductive agent consumption is little, cost is low is provided.
The present inventor finds through further investigation, in preparing the process of titanium dioxide, if passed under pressurized air stirs, in acidolysis device, directly carrying out iron powder reducing processing can cause the consumption of iron powder larger, in order to overcome this defect, contriver has stopped compressed-air actuated passing into after leaching processing finishes, and in reduction is processed, adopt other alr modes except passing into pressurized air, thereby overcome above-mentioned defect, reduce the consumption of reductive agent, thereby completed the present invention.
In addition, the present inventor infers that the reason of the consumption that can reduce reductive agent is: in the present invention, after leaching processing finishes, stop passing into described pressurized air, can prevent that thus the titanous and the ferrous iron that in reduction reaction, restore are oxidized to titanic and ferric iron again, thereby without the titanic again by reductive agent, this being oxidized to again and ferric iron, be again reduced into titanous and ferrous iron, reduced significantly thus the consumption of reductive agent.
To achieve these goals, the preparation method who the invention provides a kind of titanium dioxide, the method comprises: titaniferous material is carried out to acidolysis processing, leaching processing, reduction processing, sedimentation processing, hydrolysis treatment and calcination processing successively, wherein, in described acidolysis, process and leach in processing, in reaction system, pass into pressurized air, after leaching processing finishes, stop passing into described pressurized air, and under agitation condition, material and reductive agent after leaching is processed carry out contact reacts, wherein, and with TiO
2meter, in the material after described leaching is processed, contained titanium elements and the mol ratio of described reductive agent are 1:(0.06-0.95).
By adopting the preparation method of titanium dioxide of the present invention, after finishing in leaching processing, stopped compressed-air actuated passing into, can obtain the titanium leaching liquid that titanous concentration meets the demands with the reductive agent of lower consumption thus, thereby obtain the higher titanium dioxide of whiteness, reduced and become to produce cost, increased production efficiency.
Other features and advantages of the present invention partly in detail are described the embodiment subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation 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 to acidolysis processing, leaching processing, reduction processing, sedimentation processing, hydrolysis treatment and calcination processing successively, wherein, in described acidolysis, process and leach in processing, in reaction system, passing into pressurized air, after leaching processing finishes, stop passing into described pressurized air, and under agitation condition, material and reductive agent after leaching is processed carry out contact reacts, wherein, with TiO
2meter, in the material after described leaching is processed, contained titanium elements and the mol ratio of described reductive agent are 1:(0.06-0.95).
The present inventor also finds, because the material after acidolysis can solidify in maturing process, in acidolysis device, directly whipping appts being installed is inappropriate for suitability for industrialized production, therefore, particularly preferably, contriver is sent to the material of processing through leaching in acidolysis device in outside reducing bath, and in this reducing bath, under mechanical stirring, reduce processing, thereby thereby the defect of both successfully having avoided existing reduction to adopt pressurized air to stir in processing has reduced the consumption of iron powder or iron filings, can realize again the industrial production of serialization.What deserves to be explained is, in the present invention, although pass into compressed-air actuated object, be also in order to stir, in reduction is processed, described agitation condition does not comprise that this passes into compressed-air actuated alr mode, and it can be mechanical stirring, magnetic agitation or ultrasonic stirring.
Of the present invention a kind of preferred embodiment in, the preparation method of described titanium dioxide comprises: titaniferous material is carried out to acidolysis processing, leaching processing, reduction processing, sedimentation processing, hydrolysis treatment and calcination processing successively, wherein, described acidolysis is processed and leaching processing is to carry out in acidolysis device, and after leaching processing finishes, stop passing into described pressurized air, and the material after leaching is processed is sent in reducing bath, under mechanical stirring condition, material and reductive agent after leaching is processed carry out contact reacts, wherein, with TiO
2meter, in the material after described leaching is processed, contained titanium elements and the mol ratio of described reductive agent are 1:(0.06-0.95).The reducing bath is here be independent of acidolysis device outside, and it disposes mechanical stirring device.Adopt this preferred embodiment, not only can realize the reduction to described reductive agent consumption, can also realize the continuous industrial production of titanium dioxide, low-cost high yield.
The titanium material that common method for producing gtitanium dioxide with sulphuric acid adopts is that titanium content is ilmenite concentrate compared with high selected ilmenite and by ilmenite concentrate, is smelted titanium slag obtaining etc.Owing to having removed most of iron in titanium slag smelting process and having contained more titanous, thereby the titanium liquid after titanium slag acidolysis does not need to reduce.Therefore, in the present invention, described titaniferous material is particularly preferably the titaniferous ores that process is not smelted such as ilmenite.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 processed for the ease of acidolysis, preferably adopting screen over-size below 325 orders is titaniferous material below 15 % by weight (be about to titaniferous material and cross 325 object sieves, the coarse grained amount of not sifting out is only for 15 % by weight of the total amount of titaniferous material are following).
According to the present invention, described acidolysis is processed and can be adopted conventional acid system to prepare the acidolysis treatment process in the technique of titanium dioxide, for example, after being mixed with the sulphuric acid soln of about 90-94 % by weight, titaniferous material add the sulphuric acid soln of about 20-25 % by weight or water that the sulphuric acid soln in system is diluted to 84-86 % by weight, in dilution, liberated heat can be raised to temperature of reaction system 80-120 ℃ of left and right, and the iron at this temperature in titanium ore, magnesium, calcium etc. are in succession emitted heat temperature is raised to about 150-180 ℃ with sulfuric acid reaction is continuous mutually.The consumption of sulphuric acid soln can be adjusted according to the amount of titaniferous material and composition, and for example, the titanium of the 40-60 % by weight with respect 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.
Conventionally, in described acidolysis is processed, in order to make sulphuric acid soln and titaniferous material reaction more abundant, can pass into pressurized air and stir, for example employing passes into speed and is preferably 1000-1500m
3the pressurized air of/h; until acidolysis reaction finishes; and for example, in order to obtain the acid hydrolysate (titanyl sulfate) of more titanium; conventionally also need the material after acidolysis to be preferably incubated slaking; after insulation slaking, need to add water or dilute sulphuric acid that acid hydrolysate dilution curing in slaking is leached and carried out described leaching processing, in described leaching treating processes, also need to pass into pressurized air and (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 of the present invention is processed and leaching processing also can adopt such method to carry out.
Yet only through acidolysis, process and leach in the material after processing and contain ferric ion, in reduction is processed, main purpose is just ferric ion to be reduced to ferrous ion, produce a certain amount of trivalent titanium ion simultaneously, the titanous particle producing can guarantee that ferrous ion is no longer oxidized to ferric ion in other follow-up processing, conventionally, after reduction is processed, the content of the titanous that need to produce is more than 0.8g/L.And in the present invention, preferably, in the material after the contact reacts during described reduction is processed, the content of titanous is 0.8-2g/L.
According to the present invention, in described reduction is processed, described reductive agent can be that this area routine is being prepared titanium dioxide for reducing ferric iron and titanic reductive agent, and for example iron filings and/or iron powder, be preferably iron powder, is particularly preferably 80-200 object iron powder.
According to the present invention, describedly under agitation condition, be preferably under mechanical stirring condition, thereby more advantageously avoided the large defect of reductive agent consumption that produced by dioxygen oxidation in pressurized air whipping process.Under preferable case, with TiO
2meter, in the material that described acidolysis is processed, contained titanium elements 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 is to carry out adding after 30min in described contact reacts, particularly preferably in described contact reacts, carries out adding between 30-100min second batch reductive agent.Under preferable case, the total consumption of described reductive agent of take is 100 % by weight, and described first reductive agent 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 that described reduction is processed comprises: temperature of reaction is 55-75 ℃, and the reaction times is 80-130min.More preferably, the condition that described reduction is processed comprises: temperature of reaction is 60-70 ℃, and the reaction times is 80-100min.
In a kind of preferred implementation of the present invention, what in reduction is processed, adopt is mechanical stirring, and mechanical stirring speed is preferably 10-30rpm/min.
According to the present invention, titaniferous material is processed, leached through above-mentioned acidolysis and process and reduce after processing, more just can obtain the product of titanium dioxide through sedimentation processing, hydrolysis treatment and calcination processing.In the present invention, above-mentioned sedimentation processing, 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 obtaining by method of the present invention and titaniferous can be extracted respectively.
Wherein, described sedimentation is processed and can be adopted the acid system of this area routine to prepare the sedimentation method in titanium dioxide technique, for example described sedimentation processing can be to add certain proportion flocculation agent standing in subsider, allow solid particulate flocculating settling in titanium liquid to settling bowl bottom, its supernatant liquor is for hydrolysis treatment.
Wherein, described hydrolysis treatment can adopt the acid system of this area routine to prepare the method for hydrolysis in titanium dioxide technique, for example described hydrolysis treatment is the process that the supernatant liquor after sedimentation is processed is hydrolyzed, and the mode that can adopt automatic growing crystal species hydrolysis can be also the mode of plus seed hydrolysis.
Wherein, described calcination processing can adopt the acid system of this area routine to prepare the method for calcinating in titanium dioxide technique, for example 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 describe the present invention by embodiment.
In following examples and comparative example, the content of titanous is to adopt to take potassium sulfocyanate as indicator, by the method for ferric ammonium sulfate standardized solution titration, measures; Adopt color difference meter to detect titanium dioxide sample b value (scope of b value representation from gold-tinted to blue light, its codomain is+127 to-128 ,+127 b value representation yellow ,-128 b value representation blueness), the larger expression sample of b value is more yellow, and b value is whiter the closer to 0 value sample; Ilmenite concentrate particle was 325 object sieves, the titaniferous material below 15 % by weight of the total amount that the coarse grained amount of not sifting out is titaniferous material.
Embodiment 1
The present embodiment is for illustrating 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), (passing into speed is 1200m in reaction mass, to pass into pressurized air
3/ h), and react 25min at 160 ℃, then (now temperature is 120 ℃) after slaking 1.5h, adopts 70m
3water dilutes leaching, and the material after leaching is sent to in reducing bath, (volume of sending into the material in reducing bath is 85m
3, and with TiO
2meter, the concentration of titanium is 130g/L).Under 65 ℃, 15rpm/min mechanical stirring speed, add the 80 order iron powders of 500kg, and react 100min, yet add again the iron powder of 80kg, then react 30min, the content of the titanous in gained titanium liquid is 1.2g/L.Titanium liquid after reduction is carried out to sedimentation processing, 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 and be hydrolyzed as crystal seed, obtain metatitanic acid and after washing, in rotary kiln (top temperature is 850 ℃), calcine 4h, obtain the titanium dioxide of 9550kg, b value is 2.
Embodiment 2
The present embodiment is for illustrating 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), (passing into speed is 1400m in reaction mass, to pass into pressurized air
3/ h), and react 17min at 180 ℃, then (now temperature is 126 ℃) after slaking 2h, adopts 60m
3water dilutes leaching, and the material after leaching is sent to in reducing bath, (volume of sending into the material in reducing bath is 74m
3, and with TiO
2meter, the concentration of titanium is 135g/L).Under 70 ℃, 20rpm/min mechanical stirring speed, add the 100 order iron powders of 550kg, and react 50min, yet add again the iron powder of 75kg, then react 30min, the content of the titanous in gained titanium liquid is 1g/L.Titanium liquid after reduction is processed, 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 and be hydrolyzed as crystal seed, obtain metatitanic acid and after washing, in rotary kiln (top temperature is 950 ℃), calcine 4.5h, obtain the titanium dioxide of 9120kg, b value is 2.05.
Embodiment 3
The present embodiment is for illustrating 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), (speed of passing into is 1300m in reaction mass, to pass into pressurized air
3/ h), and react 30min at 175 ℃, then (now temperature is 100 ℃) after slaking 1h, adopts 80m
3water dilutes leaching, and the material after leaching is sent to in reducing bath, (volume of sending into the material in reducing bath is 93m
3, and with TiO
2meter, the concentration of titanium is 140g/L).Under 70 ℃, 30rpm/min mechanical stirring speed, add the 200 order iron powders of 660kg, and react 50min, yet add again the iron powder of 70kg, then react 30min, the content of the titanous in gained titanium liquid is 1.5g/L.Titanium liquid after reduction is processed, 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 and be hydrolyzed as crystal seed, obtain metatitanic acid and after washing, in rotary kiln (top temperature is 800 ℃), calcine 5h, obtain the titanium dioxide of 11450kg, b value is 1.95.
Embodiment 4
The present embodiment is for illustrating the preparation method of titanium dioxide of the present invention.
According to the method described in embodiment 1, difference is, the disposable iron powder that adds 580kg in reduction is processed, 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, reduces processing, and (speed of passing into is 350m after leaching in dilution, to continue to pass into pressurized air
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, reduces processing, and (speed of passing into is 350m after leaching in dilution, to continue to pass into pressurized air
3/ h), add iron powder 800kg, the content of the titanous in gained titanium liquid is 1.2g/L, then obtain 8632kg (titanium dioxide, its b value is 2.15.
Result by comparing embodiment and comparative example is known, adopts method of the present invention can reduce the consumption of reductive agent, obtains 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 characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, between various embodiment of the present invention, also can carry out arbitrary combination, 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 (9)
1. the preparation method of a titanium dioxide, the method comprises: titaniferous material is carried out to acidolysis processing, leaching processing, reduction processing, sedimentation processing, hydrolysis treatment and calcination processing successively, it is characterized in that, in described acidolysis, process and leach in processing, in reaction system, pass into pressurized air, after leaching processing finishes, stop passing into described pressurized air, and under agitation condition, material and reductive agent after leaching is processed carry out contact reacts, wherein, with TiO
2meter, in the material after described leaching is processed, contained titanium elements and the mol ratio of described reductive agent are 1:(0.06-0.95).
2. method according to claim 1, wherein, with TiO
2meter, in the material after described leaching is processed, contained titanium elements and the mol ratio of described reductive agent are 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 that described reduction is processed comprises: temperature of reaction is 55-75 ℃, and the reaction times is 80-130min.
6. according to the method described in any one in claim 1-5, wherein, in described reduction is processed, described reductive agent adds in two batches, first reductive agent is to add before described contact reacts, and second batch reductive agent is to carry out adding after 30min in described contact reacts.
7. method according to claim 6, wherein, the total consumption of described reductive agent of take is 100 % by weight, and described first reductive agent accounts for 80-95 % by weight, and described second batch reductive agent accounts for 5-20 % by weight.
8. according to the method described in any one in claim 1-7, wherein, in the material after described contact reacts, the content of titanous is 0.8-2g/L.
9. according to the method described in any one in claim 1-8, wherein, with TiO
2meter, in the material after described leaching is processed, the content of titanium elements is 120-140g/L.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN111646502A (en) * | 2020-06-10 | 2020-09-11 | 攀钢集团研究院有限公司 | Slag ore mixing continuous acidolysis leaching method and equipment |
| 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 |
| 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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| 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 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111646502A (en) * | 2020-06-10 | 2020-09-11 | 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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