CN102765750A - Preparation method of titanium-rich material - Google Patents
Preparation method of titanium-rich material Download PDFInfo
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- CN102765750A CN102765750A CN2012101556415A CN201210155641A CN102765750A CN 102765750 A CN102765750 A CN 102765750A CN 2012101556415 A CN2012101556415 A CN 2012101556415A CN 201210155641 A CN201210155641 A CN 201210155641A CN 102765750 A CN102765750 A CN 102765750A
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Abstract
The invention discloses a preparation method of a titanium-rich material. The method comprises the following steps: raw material crushing, pelletizing, pre-oxidation, reduction, crushing and separation. The separation step is as below: crushing a mixture of iron and titanium-rich material; then reacting the mixture with a titanium liquid generated from titanium dioxide production by a sulphuric acid method and treated with acid hydrolysis, extraction and purification; and carrying out solid-liquid separation after conversion of Fe<3+> into Fe<2+> in the titanium liquid and generation of Ti<3+>, so as to obtain a filter cake, which is the titanium-rich material. The titanium-rich material provided by the invention has a titanium dioxide content up to 80-83%; and compared with prior art, the invention has beneficial effects of low unit energy consumption and high utilization rate of resources.
Description
Technical field
The present invention relates to a kind of preparation method of rich titanium material, belong to the titanium white production field.
Background technology
The preparation method of rich titanium material is a lot, can be divided into thermal process and wet processing by production technique.Thermal process comprises electric furnace smelting process, selective chlorination, plasmamelt process etc., and wet processing comprises partial reduction-salt acid leaching process, partial reduction-sulfuric acid leaching, full reduction-rusting process etc.Electric furnace smelting process is simple and reliable, can obtain two kinds of products of rich titanium material and pig simultaneously, but power consumption is big, only limits to the competent area of electric power and uses, and fusion process mainly is to separate deironing, removes non-iron contamination ability.Pickling process is because " three wastes " amount is big, and the secondary flow journey is complicated, thereby has limited its application.Reduction corrosion rule only is applicable to handles high-grade ore in sand form.
Chinese patent 200710202160.4; Granted publication number is CN101172647B; Name is called the method for method for producing gtitanium dioxide with sulphuric acid; Disclose a kind of preparation method of rich titanium material: after ilmenite metallization reduction, first magnetic separation powder process utilizes the method for the spent acid acidolysis in the titanium white production to obtain rich titanium material then; But this method does not have the reduced iron powder in the good use rich state material production process, causes the waste of resource.
Summary of the invention
To the problems of the prior art, technical problem to be solved by this invention is that the preparation with rich titanium material combines with the production of white titanium pigment closely, and the intermediate product that makes full use of in the titanium white production prepares rich titanium material.
Technical scheme of the present invention is: a kind of preparation method of rich titanium material may further comprise the steps: raw material pulverizing, make ball; Preoxidation, reduction is pulverized; Separate; Said separating step is: with the mixture pulverizing of iron and rich titanium material, react with the titanium liquid after acidolysis, leaching, purification that Titanium White Production By Sulfuric Acid Process is produced then, treat the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the solid that obtains is rich titanium material.
Further, the liquid that obtains through solid-liquid separation is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
Further, the rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process
Further, the rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
Further, its temperature of reaction is 65 ~ 75 ℃.
The present invention makes full use of the characteristics in rich titanium material preparation and the Titanium White Production By Sulfuric Acid Process, makes the two combination tightr, utilizes the reduced iron powder that produces in the rich titanium material process of preparation to Fe
3+Reduce, can rich titanium material be separated with iron powder on the one hand, practiced thrift the use of reductive agent in the Titanium White Production By Sulfuric Acid Process on the other hand.
Content of titanium dioxide reaches 80 ~ 83% in the rich titanium material of the present invention's preparation, and compared with prior art, the present invention has the beneficial effect that unit consumption of energy is low, resource utilization is high.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 2wt%, sticker 0.5wt%, the water 5wt% of ilmenite amount, mixes, and makes ball;
3) at 600 ℃ of following preoxidation 2h;
4) with the coke be reductive agent, the coke add-on is the 20wt% of ilmenite amount, at 1200 ℃ of following reductase 12 h, obtains iron and rich titanium material mixture;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 75 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process.
Embodiment 2
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 8wt%, sticker 2wt%, the water 10wt% of ilmenite amount, mixes, and makes ball;
3) at 850 ℃ of following preoxidation 2h;
4) with the coke be reductive agent, the coke add-on is the 20wt% of ilmenite amount, at 1200 ℃ of following reductase 12 h, obtains iron and rich titanium material mixture;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 65 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process.
Embodiment 3
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 4wt%, sticker 1wt%, the water 7wt% of ilmenite amount, mixes, and makes ball;
3) at 700 ℃ of following preoxidation 1h;
4) with the coke be reductive agent, the coke add-on is the 12wt% of ilmenite amount, and reduction 1h obtains iron and rich titanium material mixture under 1100 ℃;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 70 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process.
Embodiment 4
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 6wt%, sticker 1.5wt%, the water 9wt% of ilmenite amount, mixes, and makes ball;
3) at 800 ℃ of following preoxidation 1.5h;
4) with the coke be reductive agent, the coke add-on is the 18wt% of ilmenite amount, and reduction 1.5h obtains iron and rich titanium material mixture under 1100 ℃;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 70 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process.
Embodiment 5
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 2wt%, sticker 0.5wt%, the water 5wt% of ilmenite amount, mixes, and makes ball;
3) at 600 ℃ of following preoxidation 2h;
4) with the coke be reductive agent, the coke add-on is the 20wt% of ilmenite amount, at 1200 ℃ of following reductase 12 h, obtains iron and rich titanium material mixture;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 75 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
Embodiment 6
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 8wt%, sticker 2wt%, the water 10wt% of ilmenite amount, mixes, and makes ball;
3) at 850 ℃ of following preoxidation 2h;
4) with the coke be reductive agent, the coke add-on is the 20wt% of ilmenite amount, at 1200 ℃ of following reductase 12 h, obtains iron and rich titanium material mixture;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 65 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
Embodiment 7
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 4wt%, sticker 1wt%, the water 7wt% of ilmenite amount, mixes, and makes ball;
3) at 700 ℃ of following preoxidation 1h;
4) with the coke be reductive agent, the coke add-on is the 12wt% of ilmenite amount, and reduction 1h obtains iron and rich titanium material mixture under 1100 ℃;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 70 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
Embodiment 8
A kind of preparation method of rich titanium material may further comprise the steps:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 6wt%, sticker 1.5wt%, the water 9wt% of ilmenite amount, mixes, and makes ball;
3) at 800 ℃ of following preoxidation 1.5h;
4) with the coke be reductive agent, the coke add-on is the 18wt% of ilmenite amount, and reduction 1.5h obtains iron and rich titanium material mixture under 1100 ℃;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 70 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
The rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
Above embodiment only is that the technical scheme that the present invention is put down in writing illustrates, and all simple distortion of under the situation that does not break away from core of the present invention, making or modification all fall into protection scope of the present invention.
Claims (5)
1. the preparation method of a rich titanium material may further comprise the steps: raw material pulverizing, make ball; Preoxidation, reduction is pulverized; Separate, it is characterized in that said separating step is: the mixture of iron and rich titanium material is pulverized; The Fe in the said titanium liquid is treated in the titanium liquid reaction after acidolysis, leaching, purification that is produced with Titanium White Production By Sulfuric Acid Process then
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the solid that obtains is rich titanium material.
2. the preparation method of a kind of rich titanium material according to claim 1 is characterized in that, the liquid that obtains through solid-liquid separation is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
3. the preparation method of a kind of rich titanium material according to claim 1 is characterized in that, the rich titanium material that obtains is used for the acidolysis step of Titanium White Production By Sulfuric Acid Process
4, the preparation method of a kind of rich titanium material according to claim 1 is characterized in that, the rich titanium material that obtains is used for the chlorinating step that chlorination is produced white titanium pigment.
4. the preparation method of a kind of rich titanium material according to claim 1 is characterized in that, its temperature of reaction is 65 ~ 75 ℃.
5.6, according to the preparation method of each described a kind of rich titanium material of claim 1-5, it is characterized in that this method may further comprise the steps successively:
1) ilmenite is pulverized;
2) in ilmenite powder, add Na
2CO
3, add-on is 2 ~ 8wt%, sticker 0.5 ~ 2wt%, the water 5 ~ 10wt% of ilmenite amount, mixes, and makes ball;
3) at 600 ~ 850 ℃ of following preoxidation 0.5 ~ 2h;
4) with the coke be reductive agent, the coke add-on is 8 ~ 20wt% of ilmenite amount, and reduction 0.5 ~ 2h obtains iron and rich titanium material mixture under 1000 ~ 1200 ℃;
That 5) uses that Titanium White Production By Sulfuric Acid Process produced reacts under 65 ~ 75 ℃ through the titanium liquid after acidolysis, leaching, the purification and iron and rich titanium material mixture, treats the Fe in the said titanium liquid
3+Be converted into Fe
2+, and Ti appears
3+After, through solid-liquid separation, the filter cake that obtains is rich titanium material;
6) filtrating that obtains of step 5) is delivered to the Crystallization Separation step of Titanium White Production By Sulfuric Acid Process.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103172115A (en) * | 2013-03-25 | 2013-06-26 | 山东东佳集团股份有限公司 | Method for removing ferric iron ion contained in metatitanic acid by adopting electrolytic reduction |
CN103710551A (en) * | 2014-01-15 | 2014-04-09 | 河南佰利联化学股份有限公司 | Production method of rich-titanium material |
CN104944466A (en) * | 2015-05-26 | 2015-09-30 | 河南佰利联化学股份有限公司 | Method for producing titanium-rich material by wet method |
CN105502482A (en) * | 2014-10-15 | 2016-04-20 | 刘浩 | Preparation method of titanium dioxide |
Citations (2)
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CN1114364A (en) * | 1994-06-29 | 1996-01-03 | 冶金工业部长沙矿冶研究院 | Method and equipment for producing titanium-rich material |
CN1283706A (en) * | 1999-08-10 | 2001-02-14 | 中南工业大学 | Process for preparing Ti-enriched material from ilmenite concentrate |
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2012
- 2012-05-19 CN CN2012101556415A patent/CN102765750A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1114364A (en) * | 1994-06-29 | 1996-01-03 | 冶金工业部长沙矿冶研究院 | Method and equipment for producing titanium-rich material |
CN1283706A (en) * | 1999-08-10 | 2001-02-14 | 中南工业大学 | Process for preparing Ti-enriched material from ilmenite concentrate |
Non-Patent Citations (1)
Title |
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郭宇峰等: "活化焙烧-酸浸法富集中低品位富钛料", 《中国有色金属学报》, vol. 15, no. 9, 30 September 2005 (2005-09-30) * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103172115A (en) * | 2013-03-25 | 2013-06-26 | 山东东佳集团股份有限公司 | Method for removing ferric iron ion contained in metatitanic acid by adopting electrolytic reduction |
CN103710551A (en) * | 2014-01-15 | 2014-04-09 | 河南佰利联化学股份有限公司 | Production method of rich-titanium material |
CN103710551B (en) * | 2014-01-15 | 2014-12-24 | 河南佰利联化学股份有限公司 | Production method of rich-titanium material |
CN105502482A (en) * | 2014-10-15 | 2016-04-20 | 刘浩 | Preparation method of titanium dioxide |
CN104944466A (en) * | 2015-05-26 | 2015-09-30 | 河南佰利联化学股份有限公司 | Method for producing titanium-rich material by wet method |
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Application publication date: 20121107 |