CN1923703A - Method of preparing synthetic rutile from ore type ilmenite concentrate - Google Patents
Method of preparing synthetic rutile from ore type ilmenite concentrate Download PDFInfo
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- CN1923703A CN1923703A CN 200510032102 CN200510032102A CN1923703A CN 1923703 A CN1923703 A CN 1923703A CN 200510032102 CN200510032102 CN 200510032102 CN 200510032102 A CN200510032102 A CN 200510032102A CN 1923703 A CN1923703 A CN 1923703A
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Abstract
The invention discloses an artificial rutile preparing method through rock ilmenite concentrate, which comprises the following steps: preheating rock ilmenite concentrate in the rotary kiln to reduce directly; separating the corrosion of reduced ilmenite; immersing material with titanium in the diluted acid to remove impurity to prepare the artificial rutile.
Description
Technical field
The invention belongs to the metallurgical engineering field, relate to a kind of ore type ilmenite concentrate that utilizes and be raw material, adopt reduction-rusting process to produce the method for artificial rutile.
Background technology
At present, can be used for titanium in world's titanium resource industrial mainly is natural rutile and ilmenite.But natural rutile concentrate reserves are less, and the abundant ilmenite of reserves becomes the main production raw material of titanium industry.At occurring in nature, ilmenite is divided into rock ore deposit and placer two classes, and is wherein in the majority with the rock ore deposit.The ilmenite concentrate of selecting from rock ore deposit and placer can be directly used in produces metal titanium and titanium white, but because its grade is low, generally all needs enrichment to become high-grade rich titanium material-titanium slag or artificial rutile, is used further to the production of Ti product.Relevant ilmenite is produced the research of rich titanium material method, always is titanium industrial circle one of active subject the most.The method of producing rich titanium material of having studied and having proposed mainly contains electric furnace smelting process, selective chlorination, reduction pickling process, choosing-smelting associating dilute hydrochloric acid pressure leaching process, gives oxidation-fluidization pickling process, reduction bubble method and reduction magnetic method etc.Wherein, the reduction bubble method is to be metallic iron with the ferriferous oxide in the ilmenite through solid state reduction, then with aqueous electrolyte liquid with the metallic iron corrosion in the reduced ilmenite and separate, make TiO
2Enrichment becomes artificial rutile.This method power consumption and chemical reagent amount are all few, brown coal, sub-bituminous coal with cheapness are the energy, the waste water of discharging in the corrosion process approaches neutrality (pH6～6.5), but the red mud drying is as the raw material of ironmaking, also can further be processed into the pigment-level iron oxide red, the three wastes are administered easily, have little, the advantages such as cost is low, good product quality of pollution.At present, to select factory be the raw material production artificial rutile with high-quality ilmenite placer all Australian WSL, RGC, three producers of Tiwest, east wind smeltery, domestic Zhuzhou and the North Sea.From the research and the production practice of producing artificial rutile of reduction bubble method, the reduction bubble method only is suitable for handling higher-grade placer at present, and this method still exists problems such as the reduction technique difficulty is big, the corrosion time is long.In addition, because industrial employing is the mode of operation of breeze directly into rotary kiln, thereby exist the hidden danger of ring formation of rotary kiln.
Do not see any report for the research of adopting the reduction bubble method to handle with the ore type concentrated ilmenite.
Summary of the invention
In order to realize from preparing synthetic rutile from ore type ilmenite concentrate special proposition the present invention.
The method of preparing synthetic rutile from ore type ilmenite concentrate, technical scheme of the present invention comprise that successively ore type ilmenite concentrate preheating applied to pelletizing rotary kiln directly reduces, and artificial rutile is produced in the corrosion separation of reduced ilmenite and the removal of impurities of titaniferous material dilute sulfuric acid.
1, ilmenite concentrate preheating applied to pelletizing rotary kiln directly reduces: ilmenite concentrate is allocated additive into and is made ball, and additive is a Sodium salts humic acids.Green-ball enters rotary kiln and reduces behind the drying grate drying and preheating.Drying grate drying and preheating system is: expect high 160-220mm, 150-200 ℃ of blasting drying period wind-warm syndrome, wind speed 0.8-1.0m/s, time 1-3min, down-draft drying zone wind-warm syndrome 200-250 ℃, wind speed 0.8-1.0m/s, time 4-6min, 800-950 ℃ of preheating section wind-warm syndrome, wind speed 1.0-1.2m/s, time 10-12min; The rotary kiln reduction adopts brown coal or sub-bituminous coal to make reductive agent, and reduction temperature 1100-1150 ℃, recovery time 120-150min, C/Fe is than being 0.8-0.9.
2, the corrosion of reduced ilmenite separates: to reduction gained metallized pellet carry out fragmentation, ore grinding is handled, grinding particle size is controlled at-1mm accounts for 100%, carry out the corrosion separating treatment then.The corrosion separation condition is: the corrosion agent is NH
4Cl 0.5-1.0% and HCl 1.2-2.0% mixed solution, the corrosion temperature is 60-85 ℃, and solid-to-liquid ratio is 1: 4, and stirring velocity is 400r.min
-1, air flow quantity is 1.5m
3.min
-1.t
-1 Reduced ilmenite, the corrosion time is 12-18h.Adopt screw classifier and shaking table that the ferric hydrous oxide that generates in the corrosion process is separated from the reduced ilmenite parent, red mud (ferric hydrous oxide) drying can be used as the raw material of ironmaking, also can further be processed into the pigment-level iron oxide red.
3, artificial rutile is produced in the removal of impurities of titaniferous material dilute sulfuric acid: corrosion separates back gained titaniferous material and leaches through diluted acid, further deviate from FeO, MgO, CaO, MnO etc. and remove soluble impurity, the HCl mass percent concentration is 5-8%, the acidleach solid-to-liquid ratio is 1: 4,100 ℃ of extraction temperatures, extraction time 2h, soak slag after filtration, can obtain to be used to produce the artificial rutile of chloride process titanium dioxide and titanium sponge after dry, the calcining.
Described ilmenite concentrate contains TiO
246.5-49.5%, TFe30-34%.
Described additive is a Sodium salts humic acids, and its addition is 1.0-3.0%.
The present invention has following characteristics:
(1) the present invention adopts the direct reducing process of preheating applied to pelletizing rotary kiln, go into kiln pelletizing ultimate compression strength and reach 800-1100N/, abrasion resistance index (3mm content＜3%), satisfy rotary kiln reduction requirement fully, compare with tradition reduction bubble method, the present invention helps eliminating the ring formation hidden danger of rotary kiln reducing process.
(2) additive has the effect of strengthening ilmenite reduction in the reduction process of the present invention, can reduce reduction temperature, shorten the recovery time.At reduction temperature 1100-1150 ℃, recovery time 120-150min, the C/Fe ratio is under the condition of 0.8-0.9, and degree of metalization all can reach 93-95%.
(3) the present invention separates the leaching of back gained titaniferous material employing diluted acid to corrosion, further deviates from FeO, MgO, CaO, MnO etc. and removes soluble impurity, helps guaranteeing the quality of artificial rutile product.
Description of drawings: Fig. 1: process flow diagram of the present invention.
Embodiment:
1: ore type ilmenite concentrate (TiO
247.16%, TFe31.47%) allocate additive into and make ball.The addition of additive Sodium salts humic acids is 1.5%.Green-ball is behind the drying grate drying and preheating, entering rotary kiln reduces, drying grate drying and preheating system is: expect high 200mm, 200 ℃ of blasting drying period wind-warm syndrome, wind speed 1.0m/s, time 2min, 250 ℃ of down-draft drying zone wind-warm syndrome, wind speed 1.0m/s, time 5min, 800-950 ℃ of preheating section wind-warm syndrome, wind speed 1.2m/s, time 12min; The rotary kiln reduction adopts brown coal or sub-bituminous coal to make reductive agent, 1150 ℃ of reduction temperatures, and recovery time 150min, the C/Fe ratio is 0.8, the degree of metalization of gained reduced ilmenite is 93.78%.With reduced ilmenite fragmentation, ore grinding, grinding particle size is controlled at-and 1mm accounts for 100%, carries out the corrosion separating treatment then.The corrosion separation condition is: the corrosion agent is NH
4Cl0.5% and HCl1.5% mixed solution, corrosion temperature are 70 ℃, and solid-to-liquid ratio is 1: 4, and stirring velocity is 400r.min
-1, air flow quantity is 1.5m
3.min
-1.t
-1 Reduced ilmenite, the corrosion time is 14h.Adopt screw classifier and shaking table that the ferric hydrous oxide that generates in the corrosion process is separated from the reduced ilmenite parent, the gained titaniferous material leaches through dilute hydrochloric acid, further deviate from FeO, MgO, CaO, MnO etc. and remove soluble impurity, the HCl mass percent concentration is 5-8%, the acidleach solid-to-liquid ratio is 1: 4,100 ℃ of extraction temperatures, extraction time 2h soaks slag after filtration, can obtain TiO after dry, the calcining
285.02%, the artificial rutile of the rate of recovery 90.15%.
2: ore type ilmenite concentrate (TiO
248.77%, TFe32.98%) allocate binding agent into and make ball.Binding agent Sodium salts humic acids addition is 2.5%.Green-ball is behind the drying grate drying and preheating, entering rotary kiln reduces, drying grate drying and preheating system is: expect high 180mm, 200 ℃ of blasting drying period wind-warm syndrome, wind speed 0.8m/s, time 2min, 250 ℃ of down-draft drying zone wind-warm syndrome, wind speed 0.8m/s, time 5min, 800-950 ℃ of preheating section wind-warm syndrome, wind speed 1.0m/s, time 10min; The rotary kiln reduction adopts brown coal or sub-bituminous coal to make reductive agent, 1120 ℃ of reduction temperatures, and recovery time 120min, the C/Fe ratio is 0.9, the degree of metalization of gained reduced ilmenite is 93.78%.With reduced ilmenite fragmentation, ore grinding, grinding particle size is controlled at-and 1mm accounts for 100%, carries out the corrosion separating treatment then.The corrosion separation condition is: the corrosion agent is NH
4Cl0.5% and HCl1.5% mixed solution, corrosion temperature are 75 ℃, and solid-to-liquid ratio is 1: 4, and stirring velocity is 400r.min
-1, air flow quantity is 1.5m
3.min
-1.t
-1 Reduced ilmenite, the corrosion time is 16h.Adopt screw classifier and shaking table that the ferric hydrous oxide that generates in the corrosion process is separated from the reduced ilmenite parent, the gained titaniferous material leaches through dilute hydrochloric acid, further deviate from FeO, MgO, CaO, MnO etc. and remove soluble impurity, the HCl mass percent concentration is 5-8%, the acidleach solid-to-liquid ratio is 1: 4,100 ℃ of extraction temperatures, extraction time 2h soaks slag after filtration, can obtain TiO after dry, the calcining
287.16%, the artificial rutile of the rate of recovery 90.56%.
Claims (3)
1. the method for preparing synthetic rutile from ore type ilmenite concentrate is characterized in that:
(1) the ore type concentrated ilmenite is allocated additive into and is made ball, green-ball is behind the drying grate drying and preheating, entering rotary kiln reduces, drying grate drying and preheating system is: expect high 160-220mm, 150-200 ℃ of blasting drying period wind-warm syndrome, wind speed 0.8-1.0m/s, time 1-3min, down-draft drying zone wind-warm syndrome 200-250 ℃, wind speed 0.8-1.0m/s, time 4-6min, 800-950 ℃ of preheating section wind-warm syndrome, wind speed 1.0-1.2m/s, time 10-12min; The rotary kiln reduction adopts brown coal or sub-bituminous coal to make reductive agent, and reduction temperature 1100-1150 ℃, recovery time 120-150min, C/Fe is than being 0.8-0.9;
(2) to reduction gained metallized pellet carry out fragmentation, ore grinding is handled, grinding particle size is controlled at-1mm accounts for 100%, carries out the corrosion separating treatment then, the corrosion separation condition is: the corrosion agent is NH
4Cl 0.5-1.0% and HCl 1.2-2.0% mixed solution, the corrosion temperature is 60-85 ℃, and solid-to-liquid ratio is 1: 4, and stirring velocity is 400r.min
-1, air flow quantity is 1.5m
3.min
-1.t
-1 Reduced ilmenite, the corrosion time is 12-18h;
(3) the gained titaniferous material leached through diluted acid after corrosion separated, the HCl mass percent concentration is 5-8%, and the acidleach solid-to-liquid ratio is 1: 4,100 ℃ of extraction temperatures, extraction time 2h, soak slag after filtration, can obtain to be used to produce the artificial rutile of chloride process titanium dioxide and titanium sponge after dry, the calcining.
2. method according to claim 1 is characterized in that: described ilmenite concentrate contains TiO
246.5-49.5%, TFe30-34%.
3. method according to claim 1 is characterized in that: additive therefor is a Sodium salts humic acids when making ball, and its addition is 1.0-3.0%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100321022A CN100383051C (en) | 2005-09-01 | 2005-09-01 | Method of preparing synthetic rutile from ore type ilmenite concentrate |
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|---|---|---|---|
| CNB2005100321022A CN100383051C (en) | 2005-09-01 | 2005-09-01 | Method of preparing synthetic rutile from ore type ilmenite concentrate |
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| CN1923703A true CN1923703A (en) | 2007-03-07 |
| CN100383051C CN100383051C (en) | 2008-04-23 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786082A (en) * | 2012-04-09 | 2012-11-21 | 中国科学院过程工程研究所 | Method for preparing artificial rutile |
| CN103201221A (en) * | 2010-04-06 | 2013-07-10 | 艾绿卡资源有限公司 | Improved synthetic rutile process a |
| CN103209926A (en) * | 2010-04-06 | 2013-07-17 | 艾绿卡资源有限公司 | Improved synthetic rutile process b |
| CN105256130A (en) * | 2015-10-20 | 2016-01-20 | 阿斯创钛业（营口）有限公司 | Method for recycling chloride process titanium dioxide chlorination furnace blown-out materials containing fine-grain rutile |
| CN106011501A (en) * | 2016-06-12 | 2016-10-12 | 上海大学 | Method for producing rich-titanium material by using Panzhihua ilmenite |
| CN106086478A (en) * | 2016-06-21 | 2016-11-09 | 昆明冶金研究院 | A kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material |
| CN108217722A (en) * | 2018-03-02 | 2018-06-29 | 茂名粤桥集团矿业有限公司 | A kind of raising Reductive leaching synthetic rutile TiO2The process of grade |
| CN109628762A (en) * | 2018-12-25 | 2019-04-16 | 承德市钛邦矿业有限公司 | A kind of method of wet type enrichment titanium material |
| CN112553457A (en) * | 2020-10-30 | 2021-03-26 | 河南佰利联新材料有限公司 | Method for preparing titanium-rich material from titanium middling |
| CN114790517A (en) * | 2022-03-16 | 2022-07-26 | 中南大学 | Method for preparing high-quality titanium-rich material by utilizing ilmenite |
| CN115927880A (en) * | 2022-12-30 | 2023-04-07 | 重庆大学 | Method for comprehensively utilizing ferrotitanium in titanium concentrate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69415566T2 (en) * | 1993-02-23 | 1999-07-15 | Boc Gases Australia Ltd | Process for the production of synthetic rutile |
| US6306195B1 (en) * | 2000-03-24 | 2001-10-23 | Council Of Scientific And Industiral Research | Process for the preparation of high grade synthetic rutile and pig iron |
| CN1164497C (en) * | 2001-09-15 | 2004-09-01 | 云南省冶金研究设计院 | Process for preparing artificial rutile |
| CN1225562C (en) * | 2002-10-18 | 2005-11-02 | 中国科学院过程工程研究所 | Method of producing titanium enriched material using titanium mineral |
-
2005
- 2005-09-01 CN CNB2005100321022A patent/CN100383051C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103201221A (en) * | 2010-04-06 | 2013-07-10 | 艾绿卡资源有限公司 | Improved synthetic rutile process a |
| CN103209926A (en) * | 2010-04-06 | 2013-07-17 | 艾绿卡资源有限公司 | Improved synthetic rutile process b |
| CN103201221B (en) * | 2010-04-06 | 2016-08-03 | 艾绿卡资源有限公司 | Titania method A improved |
| CN102786082A (en) * | 2012-04-09 | 2012-11-21 | 中国科学院过程工程研究所 | Method for preparing artificial rutile |
| CN105256130A (en) * | 2015-10-20 | 2016-01-20 | 阿斯创钛业（营口）有限公司 | Method for recycling chloride process titanium dioxide chlorination furnace blown-out materials containing fine-grain rutile |
| CN106011501A (en) * | 2016-06-12 | 2016-10-12 | 上海大学 | Method for producing rich-titanium material by using Panzhihua ilmenite |
| CN106086478A (en) * | 2016-06-21 | 2016-11-09 | 昆明冶金研究院 | A kind of method utilizing Yunnan ilmenite concentrate to produce reduced iron powder coproduction rich-titanium material |
| CN108217722A (en) * | 2018-03-02 | 2018-06-29 | 茂名粤桥集团矿业有限公司 | A kind of raising Reductive leaching synthetic rutile TiO2The process of grade |
| CN109628762A (en) * | 2018-12-25 | 2019-04-16 | 承德市钛邦矿业有限公司 | A kind of method of wet type enrichment titanium material |
| CN109628762B (en) * | 2018-12-25 | 2020-12-08 | 承德市钛邦矿业有限公司 | Wet titanium material enriching method |
| CN112553457A (en) * | 2020-10-30 | 2021-03-26 | 河南佰利联新材料有限公司 | Method for preparing titanium-rich material from titanium middling |
| CN114790517A (en) * | 2022-03-16 | 2022-07-26 | 中南大学 | Method for preparing high-quality titanium-rich material by utilizing ilmenite |
| CN114790517B (en) * | 2022-03-16 | 2023-10-13 | 中南大学 | Method for preparing high-quality titanium-rich material by using ilmenite |
| CN115927880A (en) * | 2022-12-30 | 2023-04-07 | 重庆大学 | Method for comprehensively utilizing ferrotitanium in titanium concentrate |
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| CN100383051C (en) | 2008-04-23 |
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