CN1710121A - Method for preparing primary titanium-rich material from high calcium-magnesium-titanium headings - Google Patents
Method for preparing primary titanium-rich material from high calcium-magnesium-titanium headings Download PDFInfo
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- CN1710121A CN1710121A CN 200510010853 CN200510010853A CN1710121A CN 1710121 A CN1710121 A CN 1710121A CN 200510010853 CN200510010853 CN 200510010853 CN 200510010853 A CN200510010853 A CN 200510010853A CN 1710121 A CN1710121 A CN 1710121A
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Abstract
The invention relates to a technique refining junior titanium-rich material with high calcium magnesium titanium fine ore. Crash titanium ore of purity 45.00 to 50.00 percent till particles of which the size is smaller than 0.074mm taking 60 to 80 percent weight, then add in with water 8 to 20 percent weight of the ore, adherent sodium silicate 3 to 5 percent, chark 10 to 20 percent, 1 to 5 percent addition sodium sulfate, 1 to 3 percent addition iron powder, 3 to 5 percent addition potassium chloride, making complex balls sized 10 to 15 mm, and acquire junior titanium-rich material after microwave drying, microwave heating and restoring, ore selecting and separating. As the titanium ore is highly wave absorptive, the heating speed is high, and the restore temperature is lowered by 80-120 deg.C, extraneous material calcium and magnesium are of good acid dissolvability which ensures the high purity of the junior titanium-rich material.
Description
(1) technical field: metallurgical technology field
(2) background technology
The production method that known ilmenite concentrate is produced primary titanium-rich material and iron powder mainly contains electric furnace smelting process, plasmamelt process, selective chlorination and other hot reducing method, partial reduction-salt acid leaching process and partial reduction-sulfuric acid leaching (general name pickling process), reduction bubble method and full reduction-HCl lixiviation process and reduction grinding method etc.Units such as Beijing Non-Ferrous Metal Research General Academy were the test that raw material has carried out artificial rutile with the Flos Bombacis Malabarici ilmenite in 1980, this method is utilized each component thermodynamic (al) difference in chlorination process in the ilmenite, control suitable mixed carbon comtent, under 900 ℃～1000 ℃ conditions selectively with the impurity chlorination, and titanium is not chlorinated, and make it to separate according to muriatic physics, chemical property, to reach enrichment TiO
2Purpose, the artificial rutile grade that this method makes is 83%, and calcium, Mg content are higher, to further reduce foreign matter content, technical difficulty is bigger, unreasonable economically, exist with a large amount of iron(ic) chloride and other by product during chlorination, be difficult to solve calcium chloride and magnesium chloride simultaneously and condense and chlorination can't be carried out in the bottom enrichment; " flotation is theoretical and select smelting to put into practice " P377-394 (metallurgical industry press, 1995.10) that beam was shown through the winter discloses a kind of " producing novel process---the reduction grinding method of rich titanium material of solubility in acid and high-quality iron powder ".The reduction temperature of tunnel furnace was 1280～1320 ℃ when this method was directly reduced, and the rich titanium material of products obtained therefrom solubility in acid is good, is suitable for the raw material as sulfate process titanium dioxide; Central South University had developed the superior production technique of ilmenite in 1999, the rich titanium material grade of producing is higher, and can further upgrade and remove calcium, impurity such as magnesium, thereby reach the grade of artificial rutile, this technology key is to make the iron grain growth in reduction process, select technology to make iron in the ilmenite become the iron powder of high added value by mill, this route will solve the frequent ring formation of rotary kiln, increase substantially the yield of mill choosing, and whether granularity satisfies problems such as the requirement (Ma Yong of titanium white chloride, the discussion of Production of Artificial Rutile route, the titanium industrial progress, 2003.3).
(3) summary of the invention
The method that the purpose of this invention is to provide a kind of preparing primary titanium-rich material from high calcium-magnesium-titanium headings, the ilmenite concentrate of grade 45.00～50.00% is added entry, binding agent, coke, composite additive after levigate, make composite pellet, separate through microwave drying, microwave heating reduction, ore dressing again and produce primary titanium-rich material.
Invention is finished according to the following steps:
1, the preparation of composite pellet: ilmenite concentrate through ore grinding to account for 60～80 weight %s of granularity less than 0.074mm, add 8%～20% water of ilmenite concentrate weight, 3～5% binding agent water glass, 10～20% cokes, 1～5% additive sulfuric acid sodium, 1～3% additive iron powder, 3～5% additive Repone K, making diameter is 10～15mm composite pellet;
2, composite pellet is through microwave drying, and drying temperature is 200-300 ℃, and be 3～15min time of drying, is dried to the composite pellet moisture content and is lower than 5 weight %;
3, place microwave oven to reduce the pelletizing after the microwave drying, processing parameter is during reduction: add the weight 40～80% that coke accounts for ilmenite concentrate, the pelletizing reduction temperature is 1150～1200 ℃, and the recovery time is 90～120min;
4, will reducing the back pelletizing, to carry out wet ball-milling to granularity be that 0.074mm accounts for 70～85 weight %, carries out magnetic separation earlier and separate, and obtains magnetic thing iron powder and nonmagnetics, and nonmagnetics carries out gravity treatment again, obtains primary titanium-rich material and carbon after the gravity treatment.Primary titanium-rich material composition TiO
260-70%, TFe 15-17.5%, SiO
24-6%, Al
2O
31-1.5%, CaO+MgO 7-11%, productive rate are more than 65%, carbon returns the pellet forming process section.
The advantage that the present invention is had compared with prior art: microwave heating belongs to the volume heating, has characteristics such as heat inside, rate of heating is fast, and ilmenite concentrate belongs to strong wave aspiration body, and heat-up rate is fast, helps enhancing productivity; With known single additive (Na
2SO
4, NaCl, Na
2CO
3) compare, reduction temperature reduces by 80 ℃～120 ℃, and impurity acid dissolubilities such as primary titanium-rich material calcium magnesium are good; The primary titanium-rich material grade can reach 60%～70%.
(4) description of drawings: Fig. 1 is a process flow sheet of the present invention.
(5) embodiment
Embodiment one
Pan Xi somewhere ilmenite concentrate composition is TFe32.18%, TiO
248.84%, CaO1.56%, MgO5.56%, SiO
25.6%, ore grinding is to the account for 60 weight %s of granularity less than 0.074mm, add 16% water of ilmenite concentrate weight, 5% binding agent water glass, 10% coke, 2% additive sulfuric acid sodium, 3% additive iron powder, 3% additive Repone K, making diameter is 10～15mm composite pellet; Pelletizing carries out microwave drying, and the power 750W of microwave drying, drying temperature are 200 ℃, and be 12min time of drying, is dried to the composite pellet moisture content and is lower than 5 weight %; Place microwave oven to reduce the pelletizing after the microwave drying, add coke and account for 40% of ilmenite concentrate weight; The pelletizing reduction temperature is 1150 ℃; Recovery time is 90min; Reduction back pelletizing carries out wet ball-milling to ore particle degree and accounts for 70% for 0.074mm weight, separates obtaining iron powder and nonmagnetics through magnetic separation, and nonmagnetics obtains primary titanium-rich material and carbon through gravity treatment, and carbon returns makes ball operation section.The nonmagnetics productive rate is 65% during magnetic separation.Resultant primary titanium-rich material grade is 67.84%.
Embodiment two
Pan Xi somewhere ilmenite concentrate composition is Tfe34.18%, TiO
246.42%, CaO2.28%, MgO5.86%, SiO
24.6%, carry out ore grinding to the account for 80 weight %s of granularity less than 0.074mm, add 20% water of ilmenite concentrate weight, 3% water glass, 18% coke, 4% sodium sulfate, 1% iron powder, 5% Repone K, making diameter is 10～15mm composite pellet; Pelletizing carries out microwave drying, the power 1000W of microwave drying, drying temperature is 300 ℃, be 3min time of drying, place microwave oven to reduce the pelletizing after the microwave drying, add coke and account for 60% of ilmenite concentrate weight, the pelletizing reduction temperature is 1120 ℃, recovery time is 120min, reduction back pelletizing carries out wet ball-milling, and being milled to granularity is that 0.074mm accounts for 85 weight %, separates obtaining iron powder and nonmagnetics through magnetic separation, nonmagnetics obtains primary titanium-rich material and carbon through gravity treatment, and carbon returns makes ball operation section.The nonmagnetics productive rate is 62% during magnetic separation, and resultant primary titanium-rich material grade is 69.12%.
Claims (3)
1, a kind of method of preparing primary titanium-rich material from high calcium-magnesium-titanium headings, ilmenite concentrate is added entry, binding agent, coke, additive after levigate, make composite pellet, again drying, add thermal reduction, ore dressing and separate and produce primary titanium-rich material, it is characterized in that: invention is finished according to the following steps:
1), the preparation of composite pellet: ilmenite concentrate through ore grinding to account for 60～80 weight %s of granularity less than 0.074mm, add 8%～20% water of ilmenite concentrate weight, 3～5% binding agent water glass, 10～20% cokes, 1～5% additive sulfuric acid sodium, 1～3% additive iron powder, 3～5% additive Repone K, making diameter is 10～15mm composite pellet;
2), composite pellet is through microwave drying, drying temperature is 200-300 ℃, be 3～15min time of drying, is dried to the composite pellet moisture content and is lower than 5 weight %;
3), place microwave oven to add thermal reduction the pelletizing after the microwave drying, add 40～80 weight % that coke accounts for ilmenite concentrate, the pelletizing reduction temperature is 1150～1200 ℃, and the recovery time is 90～120min;
4), will reducing the back pelletizing, to carry out wet ball-milling to granularity be that 0.074mm accounts for 70～85 weight %, carries out magnetic separation earlier and separate, and obtains magnetic thing iron powder and nonmagnetics, nonmagnetics carries out gravity treatment again, obtains primary titanium-rich material and carbon after the gravity treatment.
2, the method for preparing primary titanium-rich material from high calcium-magnesium-titanium headings according to claim 1 is characterized in that: the ilmenite concentrate composition is TFe 32.18%, TiO
248.84%, CaO 1.56%, MgO 5.56%, SiO
25.6%, ore grinding is to the account for 60 weight %s of granularity less than 0.074mm, 16% water that adds ilmenite concentrate weight, 5% water glass, 10% coke, 2% sodium sulfate, 3% iron powder, 3% Repone K, making diameter is 10～15mm composite pellet, the power 750W of pelletizing microwave drying, drying temperature is 200 ℃, be 12min time of drying, place microwave oven to add thermal reduction the pelletizing after the microwave drying, add coke and account for 40 weight % of ilmenite concentrate, the pelletizing reduction temperature is 1150 ℃, recovery time is 90min, it is that 0.074mm accounts for 70 weight % that reduction back pelletizing carries out wet ball-milling to granularity, separates obtaining iron powder and nonmagnetics through magnetic separation, and nonmagnetics obtains primary titanium-rich material and carbon through gravity treatment.
3, the method for preparing primary titanium-rich material from high calcium-magnesium-titanium headings according to claim 1 is characterized in that: the ilmenite concentrate composition is TFe 34.18%, TiO
246.42%, CaO 2.28%, MgO 5.86%, SiO
24.6%, carry out ore grinding to the account for 80 weight %s of granularity less than 0.074mm, 20% water that adds ilmenite concentrate weight, 3% water glass, 18% coke, 4% sodium sulfate, 1% iron powder, 5% Repone K, making diameter is 10～15mm composite pellet, the power 1000W of pelletizing microwave drying, drying temperature is 300 ℃, be 3min time of drying, place microwave oven to reduce the pelletizing after the microwave drying, add coke and account for 60% of ilmenite concentrate weight, the pelletizing reduction temperature is 1120 ℃, recovery time is 120min, it is that 0.074mm accounts for 85 weight % that reduction back pelletizing carries out wet ball-milling to granularity, separates obtaining iron powder and nonmagnetics through magnetic separation, and nonmagnetics obtains primary titanium-rich material and carbon through gravity treatment.
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| CNB2005100108534A CN100336924C (en) | 2005-06-16 | 2005-06-16 | Method for preparing primary titanium-rich material from high calcium-magnesium-titanium headings |
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| CN1710121A true CN1710121A (en) | 2005-12-21 |
| CN100336924C CN100336924C (en) | 2007-09-12 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007099315A1 (en) * | 2006-03-03 | 2007-09-07 | Anglo Operations Limited | Reduction processing of metal-containing ores in the presence of microwave and rf energy |
| CN101293220B (en) * | 2008-06-16 | 2010-04-14 | 中南大学 | Additive agent for iron-aluminum separation for high-alumina iron ore |
| CN101787407B (en) * | 2010-02-02 | 2011-07-20 | 昆明理工大学 | Method for reducing and extracting copper smelting waste slag through microwave carbon heating |
| CN102319622A (en) * | 2011-08-17 | 2012-01-18 | 昆明理工大学 | Method for improving grade of rutile through microwave pretreatment-magnetic separation combined process |
| CN102899480A (en) * | 2012-09-13 | 2013-01-30 | 太原理工大学 | Preparation method for nickel iron silicate ore powder pellet |
| CN104058450A (en) * | 2014-06-10 | 2014-09-24 | 攀枝花新中钛科技有限公司 | Preparation method for making titanium coke granules |
| CN104988307A (en) * | 2015-06-17 | 2015-10-21 | 贵州大学 | Method for comprehensively using titanium concentrate with high calcium and magnesium content |
| CN106521139A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Method for preparing high titanium slag through low temperature reduction and separation of titanium-containing iron ore |
| CN108531752A (en) * | 2018-06-13 | 2018-09-14 | 长江师范学院 | A kind of preparation method of reduction titanium |
| CN110093504A (en) * | 2019-05-15 | 2019-08-06 | 北京科技大学 | A kind of method and system using high calcium-magnesium-titanium heading preparation rich-titanium material |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4097574A (en) * | 1976-06-16 | 1978-06-27 | United States Steel Corporation | Process for producing a synthetic rutile from ilmentite |
| AUPR820301A0 (en) * | 2001-10-12 | 2001-11-01 | Rmg Services Pty. Ltd. | Treatment of a wide range of titanium oxide compounds |
| CN1164776C (en) * | 2002-04-12 | 2004-09-01 | 昆明理工大学 | Preparation of active zinc oxide from zinc dross by ultrasonic-microwave process |
| CN1227379C (en) * | 2003-06-12 | 2005-11-16 | 昆明理工大学 | Technqiue for soaking copper pyrites |
| CN1600440A (en) * | 2003-09-28 | 2005-03-30 | 攀枝花市经质矿产有限责任公司 | Manufacturing technique for refining native titanite |
-
2005
- 2005-06-16 CN CNB2005100108534A patent/CN100336924C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007099315A1 (en) * | 2006-03-03 | 2007-09-07 | Anglo Operations Limited | Reduction processing of metal-containing ores in the presence of microwave and rf energy |
| CN101293220B (en) * | 2008-06-16 | 2010-04-14 | 中南大学 | Additive agent for iron-aluminum separation for high-alumina iron ore |
| CN101787407B (en) * | 2010-02-02 | 2011-07-20 | 昆明理工大学 | Method for reducing and extracting copper smelting waste slag through microwave carbon heating |
| CN102319622A (en) * | 2011-08-17 | 2012-01-18 | 昆明理工大学 | Method for improving grade of rutile through microwave pretreatment-magnetic separation combined process |
| CN102319622B (en) * | 2011-08-17 | 2015-09-16 | 昆明理工大学 | A kind of method being improved grade of rutile by Microwave Pretreatment-magnetic separation process integration |
| CN102899480B (en) * | 2012-09-13 | 2014-10-29 | 太原理工大学 | Preparation method for nickel iron silicate ore powder pellet |
| CN102899480A (en) * | 2012-09-13 | 2013-01-30 | 太原理工大学 | Preparation method for nickel iron silicate ore powder pellet |
| CN104058450A (en) * | 2014-06-10 | 2014-09-24 | 攀枝花新中钛科技有限公司 | Preparation method for making titanium coke granules |
| CN104058450B (en) * | 2014-06-10 | 2016-02-17 | 攀枝花新中钛科技有限公司 | The granulation preparation of the burnt particle of a kind of titanium |
| CN104988307A (en) * | 2015-06-17 | 2015-10-21 | 贵州大学 | Method for comprehensively using titanium concentrate with high calcium and magnesium content |
| CN106521139A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Method for preparing high titanium slag through low temperature reduction and separation of titanium-containing iron ore |
| CN108531752A (en) * | 2018-06-13 | 2018-09-14 | 长江师范学院 | A kind of preparation method of reduction titanium |
| CN110093504A (en) * | 2019-05-15 | 2019-08-06 | 北京科技大学 | A kind of method and system using high calcium-magnesium-titanium heading preparation rich-titanium material |
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| CN100336924C (en) | 2007-09-12 |
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