CN104556218A - Preparation method of titanium dioxide - Google Patents
Preparation method of titanium dioxide Download PDFInfo
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- CN104556218A CN104556218A CN201310510583.8A CN201310510583A CN104556218A CN 104556218 A CN104556218 A CN 104556218A CN 201310510583 A CN201310510583 A CN 201310510583A CN 104556218 A CN104556218 A CN 104556218A
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Abstract
The invention relates to a preparation method of titanium dioxide in the technical field of titanium dioxide production. The preparation method comprises the following step: mixing a titanium ore acidolysis titanium solution and a high titanium slag acidolysis titanium solution in a weight ratio of 1: 2 to obtain a mixed titanium solution to prepare titanium dioxide. The titanium solution blended meets the hydrolytic requirements and the acid consumption is reduced; the steps of freezing crystallization, separation of ferrous sulfate and concentration of titanium solution are canceled, so that the cost is lowered; the content of impurities is reduced; the production flow is shortened; the capacity is improved; three waste emission is reduced, so that the environmental pollution is reduced.
Description
technical field
The present invention relates to titanium white production technical field, particularly a kind of preparation method of titanium dioxide.
background technology
It is the technology that China's titanium white powder manufacturer generally uses that sulfuric acid method titanium pigment is produced, its cardinal principle is mixed with sulfuric acid by titanium ore, reacts, obtained titanium liquid, then through sedimentation, heat filtering, crystallization, separation, essence filter, the operation such as concentrated, improve concentration and the clarity of black titanium liquid, remove ferrous iron wherein, obtain the titanium liquid meeting hydrolysis index.Along with the development of technology, external a lot of titanium white production enterprise, starts with the main raw material of of high grade, that impurity is few titanium slag as titanium white production.
Sulfate process titanium dioxide production and application titanium slag has plurality of advantages as raw material: due to the TiO of titanium slag
2of high grade, foreign matter content significantly declines, and is conducive to the raising of titanium dioxide output; The quantity of acidolysis discharging waste gas, residue, settled sludge etc. all reduces
;because iron titanium ratio is low, foreign matter content is few, and washing time and wastewater discharge also reduce; The operation such as can omit iron reduction, freezing and crystallizing in production, ferrous sulfate is separated, titanium liquid is concentrated; Acid consumption reduces, and iron filings need not be bought, freezing and concentrated expense can be saved, and greatly reduce production cost; Can the production cycle be shortened, improve output; Reduce three waste discharge, reduce the pollution to environment greatly.
Have so much advantage just because of employing titanium slag as raw material production titanium dioxide, to such an extent as to sulfate process titanium dioxide produces the raw material adopted in the world, more than halfly selects acid-dissolved titanium slag, just considers the ilmenite that employing is of high grade.But China's domestic employing titanium slag is that the producer of raw material production titanium dioxide is very few, and major cause is that acid-dissolved titanium slag method cost is higher.
summary of the invention
In order to overcome the above problems, the invention provides a kind of lower-cost use mixing acidolysis titanium liquid to prepare the method for titanium dioxide.Be engaged in titanium white production for many years, the four indices Nature comparison of titanium ore acidolysis titanium liquid and titanium slag acidolysis titanium liquid is familiar with.
Titanium ore acidolysis titanium liquid has following features: not containing Ti
3+; TiO
2content is low; F value is higher; Iron titanium ratio is higher.
Titanium slag acidolysis titanium liquid has following features: Ti
3+content is higher; TiO
2content is higher; F value is lower; Iron titanium ratio is lower.
Continuous groping experience aborning, in conjunction with the relative merits of titanium ore method and titanium slag method titanium white production, exploratory development goes out a set of new titanium white production technique voluntarily---and titanium ore acidolysis titanium liquid is mixed with titanium slag acidolysis titanium liquid, uses mixed with titanium liquid to produce qualified titanium dioxide.The present invention is achieved by the following measures:
A preparation method for titanium dioxide, mixes titanium ore acidolysis titanium liquid and titanium slag acidolysis titanium liquid according to the ratio of weight ratio 1:2, obtains containing Ti
3+for 1-5g/L, TiO
2for 185-200g/L, F value be 1.80-2.00, iron titanium ratio is the mixed with titanium liquid of 0.265-0.305, prepares titanium dioxide through hydrolysis, calcining;
Described titanium ore acidolysis titanium liquid is obtained by following methods: add sulfuric acid and titanium ore according to sour ore deposit than 1.45 ~ 1.90:1, use pressurized air homogenizing 10 ~ 15min, then initiation solution is added, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 1 ~ 5h, obstructed pressurized air during slaking, then adds leaching water, measures iron ore per ton add 2 ~ 4m by throwing ore deposit
3/ t leaches water, leaching temperature < 80 DEG C, obtains titanium ore acidolysis titanium liquid after reduction 5 ~ 6h.
Described titanium slag acidolysis titanium liquid is obtained by following methods: add sulfuric acid and titanium slag according to acid sludge than 1.55 ~ 2.00:1, use pressurized air homogenizing 10 ~ 15min, then initiation solution is added, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 2 ~ 6h, obstructed pressurized air during slaking, then adds leaching water, adds 2 ~ 4m by throwing quantity of slag titanium slag per ton
3/ t leaches water, leaching temperature < 80 DEG C, obtains titanium ore acidolysis titanium liquid after reduction 5 ~ 6h.
The sulfuric acid concentration > 92.5% added when preparing titanium ore acidolysis titanium liquid, after adding initiation solution, sulfuric acid concentration controls 80% ~ 90%.
Sulfuric acid concentration >=98% added when preparing titanium slag acidolysis titanium liquid, after adding initiation solution, sulfuric acid concentration controls 85% ~ 95%.
The compressed air pressure used is preferably >=0.3Mpa.
Use iron powder to reduce, iron powder add-on is 0-0.1t/m
3leaching liquid.
TiO in the titanium ore preferably used
2content>=45%, TiO in titanium slag
2content>=75%.
The calculation formula of described initiation solution add-on is V=(C1-C2) V1/C2
Wherein V------initiation solution dosage;
V1------sulphuric acid;
C1-------sulfuric acid concentration;
C2-------reaction acid concentration.
Owing to not containing Ti in titanium ore acidolysis titanium liquid
3+, titanium liquid presents yellow, and after blending by a certain percentage with titanium slag acidolysis titanium liquid, titanium slag acidolysis titanium liquid contains more Ti
3+if, Ti
3+after content is not enough to make mixing, titanium liquid contains Ti
3+, part iron powder reducing can be added, by the Fe in titanium ore acidolysis titanium liquid
3+be reduced to Fe
2+, remaining iron powder is by Ti
4+be reduced to Ti
3+, make titanium liquid Ti
3+content is in a rational scope.
The invention has the beneficial effects as follows:
1, the longer curing time is adopted, react fully, before ensureing leaching, solid phase reaches suitable temperature < 80 DEG C, does not pass into pressurized air during slaking, ensureing the content of the rear titanous of leaching, preventing titanous from reducing because passing into compressed air oxidation.
2, when titanium ore acidolysis titanium liquid mixes with titanium slag acidolysis titanium liquid, be main with reference to index with iron titanium ratio center line, take into account Ti simultaneously
3+, TiO
2, F value three indexs, meet hydrolysis requirement completely.
3, adopt the operations such as hybrid technology directly can save vacuum crystallization, ferrous sulfate is separated, titanium liquid is concentrated, decrease the expenditure of company at production costs such as these three operation manpowers, electric power, equipment, maintenance, steam, water, management;
After operation three operations such as 4, omission crystallization, ferrous sulfate are separated, titanium liquid is concentrated, the Production Flow Chart of whole black titanium liquid is shortened, and production capacity improves;
5, the relatively alone titanium ore of foreign matter content declines to some extent, is conducive to the raising of titanium dioxide output;
6, acid consumption reduces, and reduces production cost;
The quantity of 7, acidolysis discharging waste gas, residue, settled sludge etc. all reduces, and reduces three waste discharge, reduces the pollution to environment greatly;
8, production cost ratio is used alone titanium ore and titanium slag is all low, and the titanium dioxide quality produced, between titanium ore and titanium slag, is the titanium dioxide that a kind of cost performance is very high, has the very strong market competitiveness.
Embodiment
embodiment 1
(1) titanium ore acidolysis titanium liquid is prepared:
According to sour ore deposit than 1.45:1 add concentration 92.5% sulfuric acid 40t and containing TiO
2the titanium ore 27.6t of 45%, use pressurized air homogenizing 10 ~ 15min, compressed air pressure>=0.3Mpa, then adds 2.77t initiation solution, initiation solution adds rear sulfuric acid concentration 86.5%, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 1 ~ 5h, obstructed pressurized air during slaking, then adds leaching water, adds 2m according to throwing ore deposit amount
3/ t leaches water, leaching temperature < 80 DEG C, and with obtaining titanium ore acidolysis titanium liquid after iron powder reducing 5 ~ 6h, iron powder add-on is 0.002t/m
3leaching liquid.
(2) titanium slag acidolysis titanium liquid is prepared:
According to acid sludge than 1.55:1 add concentration 98% sulfuric acid 40t and containing TiO
2the titanium slag 25.8t of 75%, use pressurized air homogenizing 10 ~ 15min, compressed air pressure>=0.3 Mpa, then adds 2.15t initiation solution, initiation solution adds rear sulfuric acid concentration 93%, vapor pressure>=0.5Mpa, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 2 ~ 6h, obstructed pressurized air during slaking, then adds leaching water, adds 2m according to throwing ore deposit amount
3/ t leaches water, leaching temperature < 80 DEG C, and iron powder add-on is 0.03t/m
3leaching liquid, obtains titanium slag acidolysis titanium liquid after reduction 5 ~ 6h.
(3) mixed with titanium liquid is prepared
Titanium ore acidolysis titanium liquid step (2) and (3) prepared and titanium slag acidolysis titanium liquid mix according to the ratio of 1:2, obtain mixed with titanium liquid, again through conventional heat filtering, essence filter operation after the sedimentation of mixed with titanium liquid, namely the impurity removed inside titanium liquid improves the clarity of titanium liquid to utilize half frame pressure filter to filter further, then prepares titanium dioxide through routine hydrolysis, calcining process.
embodiment 2
(1) titanium ore acidolysis titanium liquid is prepared:
According to sour ore deposit than 1.90:1 add concentration 95% sulfuric acid 40t and containing TiO
2the titanium ore 21.05t of 50%, use pressurized air homogenizing 10 ~ 15min, compressed air pressure>=0.3Mpa, then adds 2.77t initiation solution, it is 86.5% that initiation solution adds rear sulfuric acid concentration, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 1 ~ 5h, obstructed pressurized air during slaking, then adds leaching water, adds 4m according to throwing ore deposit amount
3/ t leaches water, leaching temperature < 80 DEG C.
(2) titanium slag acidolysis titanium liquid is prepared:
According to acid sludge than 2.00:1 add concentration 98% sulfuric acid 40t and containing TiO
2the titanium slag 20t of 80%, use pressurized air homogenizing 10 ~ 15min, compressed air pressure>=0.3 Mpa, then adds 2.15t initiation solution, it is 93% that initiation solution adds rear sulfuric acid concentration, vapor pressure>=0.5Mpa, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 2 ~ 6h, obstructed pressurized air during slaking, then adds leaching water, adds 4m according to throwing ore deposit amount
3/ t leaches water, leaching temperature < 80 DEG C, and iron powder add-on is 0.1t/m
3leaching liquid, obtains titanium slag acidolysis titanium liquid after reduction 5 ~ 6h.
(3) mixed with titanium liquid is prepared
Titanium ore acidolysis titanium liquid step (2) and (3) prepared and titanium slag acidolysis titanium liquid mix according to the ratio of 1:2, obtain containing Ti
3+for 5g/L, TiO
2for 200g/L, F value be 2.0, iron titanium ratio be 0.265 mixed with titanium liquid, again through conventional heat filtering, essence filter operation after the sedimentation of mixed with titanium liquid, namely the impurity removed inside titanium liquid improves the clarity of titanium liquid to utilize half frame pressure filter to filter further, then prepares titanium dioxide through routine hydrolysis, calcining process.
Claims (8)
1. a preparation method for titanium dioxide, is characterized in that titanium ore acidolysis titanium liquid and titanium slag acidolysis titanium liquid to mix according to the ratio of weight ratio 1:2, obtains containing Ti
3+for 1-5g/L, TiO
2for 185-200g/L, F value be 1.80-2.00, iron titanium ratio is the mixed with titanium liquid of 0.265-0.305, prepares titanium dioxide through hydrolysis, calcining.
2. preparation method according to claim 1, it is characterized in that titanium ore acidolysis titanium liquid is obtained by following methods: add sulfuric acid and titanium ore according to sour ore deposit than 1.45 ~ 1.90:1, use pressurized air homogenizing 10 ~ 15min, then add initiation solution, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 1 ~ 5h, obstructed pressurized air during slaking, then add leaching water, measure iron ore per ton by throwing ore deposit and add 2 ~ 4m
3/ t leaches water, leaching temperature < 80 DEG C, obtains titanium ore acidolysis titanium liquid after reduction 5 ~ 6h.
3. preparation method according to claim 1, it is characterized in that titanium slag acidolysis titanium liquid is obtained by following methods: add sulfuric acid and titanium slag according to acid sludge than 1.55 ~ 2.00:1, use pressurized air homogenizing 10 ~ 15min, then add initiation solution, by steam heating initiation reaction, kick off temperature 80 ~ 120 DEG C, after having reacted, slaking 2 ~ 6h, obstructed pressurized air during slaking, then add leaching water, add 2 ~ 4m by throwing quantity of slag titanium slag per ton
3/ t leaches water, leaching temperature < 80 DEG C, obtains titanium ore acidolysis titanium liquid after reduction 5 ~ 6h.
4. preparation method according to claim 2, it is characterized in that the sulfuric acid concentration > 92.5% added, after adding initiation solution, sulfuric acid concentration controls 80% ~ 90%.
5. preparation method according to claim 3, is characterized in that sulfuric acid concentration >=98% added, and after adding initiation solution, sulfuric acid concentration controls 85% ~ 95%.
6. the preparation method according to Claims 2 or 3, is characterized in that compressed air pressure >=0.3Mpa.
7. the preparation method according to Claims 2 or 3, it is characterized in that using iron powder to reduce, iron powder add-on is 0-0.1t/m
3leaching liquid.
8. the preparation method according to Claims 2 or 3, is characterized in that TiO in titanium ore
2content>=45%, TiO in titanium slag
2content>=75%.
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|---|---|---|---|
| CN201310510583.8A CN104556218A (en) | 2013-10-26 | 2013-10-26 | Preparation method of titanium dioxide |
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|---|---|---|---|
| CN201310510583.8A CN104556218A (en) | 2013-10-26 | 2013-10-26 | Preparation method of titanium dioxide |
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Cited By (9)
| 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 |
| CN106241868A (en) * | 2016-08-31 | 2016-12-21 | 攀枝花大互通钛业有限公司 | A kind of titanium dioxide and preparation method thereof |
| 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 |
| CN106966427A (en) * | 2017-03-14 | 2017-07-21 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN107540015A (en) * | 2017-09-26 | 2018-01-05 | 攀钢集团研究院有限公司 | The mixed method of rich-titanium material titanium liquid and poor titanium material titanium liquid in sulfate process titanium dioxide production |
| CN108002440A (en) * | 2017-11-30 | 2018-05-08 | 广西雅照钛白有限公司 | A kind of novel production process of titanium dioxide powder |
| CN109467122A (en) * | 2019-01-10 | 2019-03-15 | 山东道恩钛业有限公司 | A kind of novel sulfuric acid process titanium dioxide acid hydrolysis method |
| CN110817951A (en) * | 2019-12-04 | 2020-02-21 | 龙佰四川钛业有限公司 | Titanium liquid concentration end point control method |
| CN114408967A (en) * | 2021-12-28 | 2022-04-29 | 龙佰襄阳钛业有限公司 | Acidolysis process for high-impurity titanium concentrate |
-
2013
- 2013-10-26 CN CN201310510583.8A patent/CN104556218A/en active Pending
Cited By (12)
| 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 |
| CN106241868A (en) * | 2016-08-31 | 2016-12-21 | 攀枝花大互通钛业有限公司 | A kind of titanium dioxide and preparation method thereof |
| CN106966427A (en) * | 2017-03-14 | 2017-07-21 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN106966427B (en) * | 2017-03-14 | 2019-10-08 | 襄阳龙蟒钛业有限公司 | The purification method of a kind of acidolysis titanium liquid and for the filter in method |
| CN107540015A (en) * | 2017-09-26 | 2018-01-05 | 攀钢集团研究院有限公司 | The mixed method of rich-titanium material titanium liquid and poor titanium material titanium liquid in sulfate process titanium dioxide production |
| CN108002440A (en) * | 2017-11-30 | 2018-05-08 | 广西雅照钛白有限公司 | A kind of novel production process of titanium dioxide powder |
| CN109467122A (en) * | 2019-01-10 | 2019-03-15 | 山东道恩钛业有限公司 | A kind of novel sulfuric acid process titanium dioxide acid hydrolysis method |
| CN109467122B (en) * | 2019-01-10 | 2020-11-06 | 山东道恩钛业有限公司 | Novel sulfuric acid method titanium dioxide acidolysis method |
| CN110817951A (en) * | 2019-12-04 | 2020-02-21 | 龙佰四川钛业有限公司 | Titanium liquid concentration end point control method |
| CN114408967A (en) * | 2021-12-28 | 2022-04-29 | 龙佰襄阳钛业有限公司 | Acidolysis process for high-impurity titanium concentrate |
| CN114408967B (en) * | 2021-12-28 | 2023-12-12 | 龙佰襄阳钛业有限公司 | Acidolysis process of high-impurity titanium concentrate |
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