CN104561606A - Clean technological method for preparing high-grade rich-titanium material by ilmenite - Google Patents
Clean technological method for preparing high-grade rich-titanium material by ilmenite Download PDFInfo
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Abstract
The invention discloses a clean technological method for preparing a high-grade rich-titanium material by ilmenite. The method comprises the following steps: (1) reducing the ilmenite by a reducing agent to obtain a reduction material containing rutile type titanium dioxide and iron; (2) separating the reduction material obtained in the step (1) to obtain the rich-titanium material and tailings. The technological method provided by the invention can be used for realizing the efficient enrichment of titanium; in the obtained rich-titanium material, the grade of the rutile type titanium dioxide is greater than 93% and the yield of the titanium is greater than 90%.
Description
Technical field
The invention belongs to chemical industry and field of metallurgy, particularly relate to a kind of clean process method utilizing ilmenite to prepare the rich titanium material of higher-grade.
Background technology
The titanium ore of about more than 90% is for the production of titanium white in the world, and the ilmenite of about 4% ~ 5% is used for metal smelting titanium, and all the other titanium ores are for the manufacture of titanium alloy, carbide, pottery, glass, welding rod and chemical etc.China's titanium resource storage capacity is very abundant, and main existence form is ilmenite, and rutile ore is very few.The titanium ore of China is mainly distributed in the ground such as Sichuan, Yunnan, Hainan, Guangdong, Guangxi, and after exploitation, main products is concentrated ilmenite, also has a little rutile concentrate.
Because in ilmenite concentrate, the grade of titanium dioxide is lower, often need after enrichment process, obtain high-grade rich titanium material-titanium slag or artificial rutile, the content of titanium dioxide in rich titanium material is made to reach 80% ~ 90%, further could apply, such as, be used as the raw materials for production of preparing titanium white through chlorination process powder.In the rich titanium material of chloride process titanium dioxide manufacturing technique requirent, the content of titanium dioxide is more than 90%, impurity (CaO+MgO)≤1.5%.When the rich titanium material of process preparation is carried out to ilmenite and titanium slag, generally select the carbonaceous material such as hard coal, coke as reductive agent, gained rich titanium material quality is difficult to reach requirement, as described in CN 103898264A invention, adopt carbonaceous material coal as reductive agent, but also there is environmental pollution to a certain extent, energy consumption is high, effective utility of laser power is low problem.
In order to realize preparing rich titanium material by the less energy-consumption of ilmenite cleanliness without any pollution, CN 103031433A proposes a kind of concentrated ilmenite fluidization oxidizing roasting-fluidized reduction roasting system and sinter process, find the ilmenite after preoxidation, again when reductive agent reduces, can reduction temperature be reduced, but have that operation is various, energy-intensive problem simultaneously.
Summary of the invention
The deficiency of rich titanium material manufacturing technique is prepared in order to overcome existing ilmenite, the object of the present invention is to provide a kind of clean process method utilizing ilmenite low-temperature reduction to prepare the rich titanium material of higher-grade, it has reduction process cleanliness without any pollution, reduction temperature is low, energy consumption is low, in reduction process, the degree of metalization of iron is high, separating effect is thorough, gained rich titanium material grade of titanium dioxide up to more than 90% feature.
For reaching above-mentioned object, the present invention adopts following technical scheme:
Reduced ilmenite prepares a clean process method for the rich titanium material of higher-grade, comprises the following steps:
(1) ilmenite is after reductive agent reduction, obtains the reducing material containing rutile titanium dioxide and fe;
(2) by step (1) gained reducing material, after being separated, rich titanium material and tailings is obtained.
As optimal technical scheme, method of the present invention, described in step (1), ilmenite is through ball milling, screening, reduction.
Preferably, the granularity after screening is less than 74 μm.
Preferably, described reductive agent is gaseous reducing agent, is preferably carbon monoxide, ammonia, hydrogen, methane, Sweet natural gas, coal gas one or more gas mixture wherein, the one more preferably in carbon monoxide, hydrogen or its gas mixture, more preferably hydrogen.
Preferably, the temperature of described reduction is 600 DEG C-1200 DEG C, such as 630 DEG C, 700 DEG C, 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C, 950 DEG C, 1000 DEG C, 1150 DEG C etc., is preferably 700 DEG C-1000 DEG C, more preferably 750 DEG C-950 DEG C; The time 30min-7h of described reduction, as 30min, 45min, 1h, 1.5h, 3h, 5h, 6.5h etc., preferred 3h-4h.
Reductive agent selected in reduction process of the present invention, reduction temperature and recovery time, free of contamination process can be realized, have the advantages that reduction temperature is low, the recovery time is short, achieve the object that energy consumption is low, capacity usage ratio is high, gained reducing material is rutile titanium dioxide and fe, in reduction process, the degree of metalization of iron is high, thus can obtain higher yield and the grade of Geng Gao when making separation.
As optimal technical scheme, method of the present invention, the method be separated described in step (2) is flotation, magnetic separation, acid-soluble, molten point, any one in corrosion, is preferably magnetic separation, acid-soluble, molten point, any one in corrosion.
Preferably, in described acid-soluble partition method, acid used is hydrochloric acid and/or sulfuric acid, is preferably hydrochloric acid.
Preferably, in described acid-soluble partition method, sour massfraction is 5%-30%, such as, be 5%, 10%, 12%, 15%, 18%, 20%, 25%, 28%, 30% etc., is preferably 5%-25%, more preferably 10%-20%.
Preferably, in described acid-soluble partition method, reducing material is 1:1-1:8, such as 1:1,1:2,1:3,1:4,1:6 etc. with the solid-liquid mass ratio of acid, is preferably 1:2-1:6, more preferably 1:3-1:5.
Preferably, the acid-soluble temperature in described acid-soluble partition method is 20 DEG C-100 DEG C, such as 20 DEG C, 25 DEG C, 40 DEG C, 60 DEG C, 80 DEG C, 100 DEG C etc., is preferably 20 DEG C-80 DEG C, more preferably 20 DEG C-60 DEG C; The acid-soluble time is 30min-10h, and such as, 30min, 1h, 2h, 4h, 8h, 10h etc., be preferably 30min-6h, more preferably 1h-4h.
By acid-soluble partition method, titanium dioxide yield is high, can obtain high-grade rich titanium material simultaneously.
Preferably, in described magnetic separating method, reducing material is through broken, ball-milling processing, and the reducing material granularity after preferably treatment is less than 74 μm.
Preferably, described magnetic separation is separated into two stages of magnetic separation, and one section of magneticstrength is 0.01T-0.4T, is preferably 0.1T-0.3T, more preferably 0.15T-0.2T; Two sections of magneticstrengties are 0.3T-1.2T, are preferably 0.4T-1.0T, more preferably 0.4T-0.8T.
By magnetic separation partition method, high-grade rich titanium material can be obtained, simple to operation, flow process is short, pollution-free.
Preferably, in described molten point method, molten point temperature is 1400 DEG C-1800 DEG C, such as 1400 DEG C, 1500 DEG C, 1550 DEG C, 1600 DEG C, 1650 DEG C, 1700 DEG C, 1750 DEG C, 1800 DEG C etc., is preferably 1500 DEG C-1650 DEG C; The time of described molten point is 1h-10h, as 2h, 3h, 4h, 6h, 8h, 10h etc., is preferably 2h-8h, is more preferably 2h-6h.
Preferably, in described molten point method, additional mixed carbon comtent is the 3%-10% of reducing material quality, such as, be 4%, 5.5%, 7%, 8.6%, 9.8% etc., preferably 5%-8%.
Preferably, in described corrosion partition method, corrosion agent is NH
4the aqueous solution of Cl or NH
4the hydrochloric acid soln of Cl, preferred NH
4the hydrochloric acid soln of Cl.
Preferably, described NH
4nH in the aqueous solution of Cl
4cl massfraction is 0.2%-0.8%, is preferably 0.4%-0.6%.
Preferably, described NH
4nH in the hydrochloric acid soln of Cl
4cl massfraction is 0.2%-0.8%, such as, be 0.3%, 0.5%, 0.7% etc., is preferably 0.4%-0.6%; HCl massfraction is 0.5%-3%, is preferably 1%-2%.
Preferably, the temperature of described corrosion is 20 DEG C-90 DEG C, such as, be 30 DEG C, 50 DEG C, 66 DEG C, 78 DEG C, 89 DEG C etc., preferably 65 DEG C-80 DEG C; The time of described corrosion is 6h-15h, preferred 6h-12h.
Compared with prior art scheme, the present invention has following beneficial effect:
(1) reduction process capacity usage ratio is high, energy consumption is low, cleanliness without any pollution.
(2) degree of metalization of reduction process iron is high: degree of metalization is greater than 95%.
(3) whole process titanium yield is high, and the rich titanium material of gained is of high grade: in rich titanium material, rutile titanium dioxide grade is greater than 93%, and whole process titanium yield is greater than 90%.
It is low that processing method of the present invention has energy consumption, and capacity usage ratio is high, cleanliness without any pollution, and the sepn process titanium dioxide rate of recovery is high, grade high.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, below the present invention is described in more detail.But following embodiment is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
Typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
The ilmenite Ti 27.67wt% that the present embodiment uses, TFe 22.91wt%, Si 2.09wt%, Al 0.91wt%, Mg 0.78wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 750 DEG C, pass into hydrogen reducing 5h, obtain reducing material.
(2) reducing material and massfraction are the hydrochloric acid of 20% is that 1:3 mixes according to solid-liquid mass ratio, and acid-soluble 4h at 95 DEG C, obtains rich titanium material after solid-liquor separation, drying.
After testing and calculate, the grade of gained rich titanium material rutile titanium dioxide is 93.96%, and the rate of recovery of whole process titanium is 98.33%.
Embodiment 2
The ilmenite Ti 37.91wt% that the present embodiment uses, TFe 13.28wt%, Si 0.928wt%, Al1.27wt%, Mn 0.795wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 850 DEG C, hydrogen reducing 4h, obtains reducing material.
(2) hydrochloric acid of reducing material and 15% massfraction is that 1:4 mixes according to solid-liquid mass ratio, and acid-soluble 3h at 20 DEG C, obtains rich titanium material after solid-liquor separation, drying.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 96.86%, and the rate of recovery of whole process titanium is 97.16%.
Embodiment 3
The ilmenite Ti 42.43wt% that the present embodiment uses, TFe 10.164wt%, Si 0.952wt%, Al0.951wt%, Mn 0.44wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 950 DEG C, hydrogen reducing 2h, obtains reducing material.
(2) hydrochloric acid of reducing material and 10% massfraction is that 1:3 mixes according to solid-liquid mass ratio, and acid-soluble 2h at 40 DEG C, obtains rich titanium material after solid-liquor separation, drying.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 94.88%, and the rate of recovery of whole process titanium is 96.37%.
Embodiment 4
The ilmenite Ti 27.67wt% that the present embodiment uses, TFe 22.91wt%, Si 2.09wt%, Al 0.91wt%, Mg 0.78wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 1000 DEG C, pass into Carbon monoxide reduction 7h, obtain reducing material.
(2) reducing material and massfraction are the sulfuric acid of 20% is that 1:4 mixes according to solid-liquid mass ratio, and acid-soluble 5h at 75 DEG C, obtains rich titanium material after solid-liquor separation, drying.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 96.26%, and the rate of recovery of whole process titanium is 97.53%.
Embodiment 5
The ilmenite Ti 37.91wt% that the present embodiment uses, TFe 13.28wt%, Si 0.928wt%, Al1.27wt%, Mn 0.795wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 1000 DEG C, under hydrogen and Co mixed gas, reduce 6h, obtain reducing material.
(2) hydrochloric acid of reducing material and 15% massfraction is that 1:5 mixes according to solid-liquid mass ratio, and acid-soluble 2h at 50 DEG C, obtains rich titanium material after solid-liquor separation, drying.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 97.36%, and the rate of recovery of whole process titanium is 98.15%.
Embodiment 6
The ilmenite Ti 37.91wt% that the present embodiment uses, TFe 13.28wt%, Si 0.928wt%, Al1.27wt%, Mn 0.795wt%.
(1) get the ilmenite of 100g, be laid in material boat, put into tube furnace, at 800 DEG C after hydrogen reducing 4h, obtain reducing material.
(2) reducing material ball milling screen less than 74 μm account for 96%, one section of magneticstrength is 0.15T, and two sections of magneticstrengties are 0.8T, solid-liquid separation, and drying obtains rich titanium material.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 93.59%, and the rate of recovery of whole process titanium is 92.82%.
Embodiment 7
The ilmenite Ti 37.91wt% that the present embodiment uses, TFe 13.28wt%, Si 0.928wt%, Al1.27wt%, Mn 0.795wt%.
(1) get the ilmenite of 500kg, reduce in electrothermic type rotary reduction furnace, adopt hydrogen as reductive agent, reduction temperature is 850 DEG C, and the recovery time is 5h, obtains reducing material.
(2) reducing material mixes with the carbon of reducing material quality 5%, and melting 6h under the high temperature of 1650 DEG C, obtains titanium slag and half iron.
After testing and calculate, the grade of gained rich titanium material titanium dioxide is 94.73%, and the rate of recovery of whole process titanium is 96.33%.
Embodiment 8
The ilmenite Ti 27.67wt% that the present embodiment uses, TFe 22.91wt%, Si 2.09wt%, Al 0.91wt%, Mg 0.78wt%.
(1) get 500kg ilmenite, reduce in steel belt type reducing furnace, at 900 DEG C, hydrogen reducing time 4h, obtains reducing material.
(2) reducing material is after being milled to granularity and being less than 1mm, at NH
4cl massfraction is 0.5%, in the corrosion solution of HCl massfraction 1.5%, 80 DEG C of process 9h, obtain rich titanium material and mud after solid-liquor separation.
After testing and calculate, the grade of gained rich titanium material rutile titanium dioxide is 93.68%, and the rate of recovery of whole process titanium is 97.36%.
As can be seen from the above embodiments, the inventive method has reduction process cleanliness without any pollution, reduction temperature is low, and energy consumption is low, and the degree of metalization of reduction process iron is high, and separation method is simple, and separating effect is thorough, the feature that gained rutile titanium dioxide is of high grade.
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, and namely unexpectedly position the present invention and must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
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 characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, 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 (10)
1. reduced ilmenite prepares a clean process method for the rich titanium material of higher-grade, comprises the following steps:
(1) ilmenite is after reductive agent reduction, obtains the reducing material containing rutile titanium dioxide and fe;
(2) by step (1) gained reducing material, after being separated, rich titanium material and tailings is obtained.
2. method according to claim 1, is characterized in that, described in step (1), ilmenite is through ball milling, screening, reduction;
Preferably, the granularity after screening is less than 74 μm.
3. method according to claim 1 and 2, it is characterized in that, described in step (1), reductive agent is gaseous reducing agent, be preferably carbon monoxide, ammonia, hydrogen, methane, Sweet natural gas, coal gas one or more gas mixture wherein, one more preferably in carbon monoxide, hydrogen or its gas mixture, more preferably hydrogen;
Preferably, the temperature of described reduction is 600 DEG C-1200 DEG C, is preferably 700 DEG C-1000 DEG C, more preferably 750 DEG C-950 DEG C; The time 30min-7h of described reduction, is preferably 3h-4h.
4. the method according to any one of claim 1-3, it is characterized in that, the method be separated described in step (2) is flotation, magnetic separation, acid-soluble, molten point, any one in corrosion, be preferably magnetic separation, acid-soluble, molten point, corrosion any one.
5. method according to claim 4, is characterized in that, in described acid-soluble partition method, acid used is hydrochloric acid and/or sulfuric acid, is preferably hydrochloric acid;
Preferably, in described acid-soluble partition method, sour massfraction is 5%-30%, is preferably 5%-25%, more preferably 10%-20%;
Preferably, in described acid-soluble partition method, reducing material is 1:1-1:8 with the solid-liquid mass ratio of acid, is preferably 1:2-1:6, more preferably 1:3-1:5.
6. the method according to claim 4 or 5, is characterized in that, the acid-soluble temperature in described acid-soluble partition method is 20 DEG C-100 DEG C, is preferably 20 DEG C-80 DEG C, more preferably 20 DEG C-60 DEG C; The acid-soluble time is 30min-10h, is preferably 30min-6h, more preferably 1h-4h.
7. method according to claim 4, is characterized in that, in described magnetic separating method, reducing material is through broken, ball-milling processing, and the reducing material granularity after preferably treatment is less than 74 μm;
Preferably, described magnetic separation is separated into two stages of magnetic separation, and one section of magneticstrength is 0.01T-0.4T, is preferably 0.1T-0.3T, more preferably 0.15T-0.2T; Two sections of magneticstrengties are 0.3T-1.2T, are preferably 0.4T-1.0T, more preferably 0.6T-0.8T.
8. method according to claim 4, is characterized in that, in described molten point method, molten point temperature is 1400 DEG C-1800 DEG C, is preferably 1500 DEG C-1650 DEG C; The time of described molten point is 1h-10h, is preferably 2h-8h, is more preferably 2h-6h;
Preferably, in described molten point method, additional mixed carbon comtent is the 3%-10% of reducing material quality, is preferably 5%-8%.
9. method according to claim 4, is characterized in that, in described corrosion partition method, corrosion agent is NH
4the aqueous solution of Cl or NH
4the hydrochloric acid soln of Cl, preferred NH
4the hydrochloric acid soln of Cl;
Preferably, described NH
4nH in the aqueous solution of Cl
4cl massfraction is 0.2%-0.8%, is preferably 0.4%-0.6%;
Preferably, described NH
4nH in the hydrochloric acid soln of Cl
4cl massfraction is 0.2%-0.8%, is preferably 0.4%-0.6%; HCl massfraction is 0.5%-3%, is preferably 1%-2%.
10. the method according to claim 4 or 9, is characterized in that, the temperature of described corrosion is 20 DEG C-90 DEG C, is preferably 65 DEG C-80 DEG C; The time of described corrosion is 6h-15h, is preferably 6h-12h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597413A (en) * | 2017-09-25 | 2018-01-19 | 攀钢集团矿业有限公司 | A kind of ilmenite beneficiation method |
| CN108384950A (en) * | 2018-04-18 | 2018-08-10 | 攀钢集团研究院有限公司 | The method of smelting titanium slag |
| CN108531752A (en) * | 2018-06-13 | 2018-09-14 | 长江师范学院 | A kind of preparation method of reduction titanium |
| CN109205665A (en) * | 2018-11-21 | 2019-01-15 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of the dedicated titanium slag of welding rod |
| CN110191967A (en) * | 2016-11-23 | 2019-08-30 | 环境清洁技术有限公司 | Via the low temperature direct-reduction of the metal oxide in situ for generating reducibility gas |
| CN110747330A (en) * | 2019-11-27 | 2020-02-04 | 宜宾天原海丰和泰有限公司 | Method for preparing chloridizable titanium-rich material by reducing ilmenite |
| CN114293031A (en) * | 2022-01-10 | 2022-04-08 | 广东粤桥新材料科技有限公司 | Multistage-type rusting method applied to iron-containing minerals |
| 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 |
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| 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 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110191967A (en) * | 2016-11-23 | 2019-08-30 | 环境清洁技术有限公司 | Via the low temperature direct-reduction of the metal oxide in situ for generating reducibility gas |
| CN107597413A (en) * | 2017-09-25 | 2018-01-19 | 攀钢集团矿业有限公司 | A kind of ilmenite beneficiation method |
| CN107597413B (en) * | 2017-09-25 | 2019-09-03 | 攀钢集团矿业有限公司 | A kind of ilmenite beneficiation method |
| CN108384950A (en) * | 2018-04-18 | 2018-08-10 | 攀钢集团研究院有限公司 | The method of smelting titanium slag |
| CN108531752A (en) * | 2018-06-13 | 2018-09-14 | 长江师范学院 | A kind of preparation method of reduction titanium |
| CN109205665A (en) * | 2018-11-21 | 2019-01-15 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of the dedicated titanium slag of welding rod |
| CN110747330A (en) * | 2019-11-27 | 2020-02-04 | 宜宾天原海丰和泰有限公司 | Method for preparing chloridizable titanium-rich material by reducing ilmenite |
| CN114293031A (en) * | 2022-01-10 | 2022-04-08 | 广东粤桥新材料科技有限公司 | Multistage-type rusting method applied to iron-containing minerals |
| 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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Application publication date: 20150429 |