CN102531048A - Method for preparing acid-soluble titanium slag by reduction at low temperature - Google Patents
Method for preparing acid-soluble titanium slag by reduction at low temperature Download PDFInfo
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- CN102531048A CN102531048A CN2012100409315A CN201210040931A CN102531048A CN 102531048 A CN102531048 A CN 102531048A CN 2012100409315 A CN2012100409315 A CN 2012100409315A CN 201210040931 A CN201210040931 A CN 201210040931A CN 102531048 A CN102531048 A CN 102531048A
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Abstract
The invention relates to a method for preparing acid-soluble titanium slag by reduction at low temperature, and belongs to the technical field of the preparation of chemical materials. The method comprises the following steps of: mixing ilmenite, carbon powder, a bonding agent and sodium carbonate, reducing, performing water cooling, crushing, and separating titanium from iron to prepare the acid-soluble titanium slag. According to the method, the ilmenite is reduced at the low temperature, so that the defect of the conventional method for separating the titanium from the iron in the ilmenite in high energy consumption is overcome, and energy consumption is reduced; due to the adoption of a tunnel kiln, ultra-high investment for constructing equipment for blast-furnace smelting and rotary hearth furnace smelting is avoided; and the comprehensive utilization of resources is implemented, and heat in the reduction process is recovered to the production to reduce production cost.
Description
Technical field
The present invention relates to the method that a kind of low-temperature reduction prepares acid-dissolved titanium slag, belong to technical field of chemical material preparation.
Background technology
Acid-dissolved titanium slag is one of important raw and processed materials of producing white titanium pigment, is used in the production field of method for producing gtitanium dioxide with sulphuric acid widely.YB/T5285-2007 is divided into three models to acid-dissolved titanium slag; Wherein the content of titanium dioxide in the TZ74 type requirement acid-dissolved titanium slag is in 72~76% scope, and the content of titanous is less than 18%, and the content of iron protoxide is less than 7%; The content of sulphur is less than 0.12%, and the content of phosphorus is less than 0.02%.
CN01128856.6 discloses a kind of isolating method of ilmenite, under vacuum condition, earlier in the plasma heating furnace with 1600~23000 ℃ of ilmenite powder addings; Make its gasification, get into 24000~40000 ℃ induction furnace again, the electronic shell of each composition molecule is separated; Obtain isolating material; Get into water cooler again, at last mixed powder is sent into separator separates, and isolated oxygen is taken away.
CN101619371 discloses a kind of method that reclaims the vanadium ferrotianium from vanadium titano-magnetite; Technological process comprises that breeze, coal dust with the sticker agglomeration, at rotary hearth furnace reduction, obtain metallized product; Hot charging gets into the furnace melting separation then, obtains vanadium-bearing hot metal and titanium oxide TiO
2>50% titanium slag.Vanadium-bearing hot metal is blown vanadium obtain vanadium slag, half steel is in converter steelmaking; Can be with titanium slag directly as the raw material of carrying titanium.
The method for preparing at present acid-dissolved titanium slag mainly is pyrotic smelting; Adopt the production technology of " blast furnace-converter " to carry out exactly; What this kind method obtained is the titanium slag that contains titanium oxide about 50%, but wherein impurity iron, vanadium etc. are still higher, and Application Areas is very narrow.
Summary of the invention
The purpose of this invention is to provide the method that a kind of low-temperature reduction prepares acid-dissolved titanium slag; This method not only can make full use of the heat in the reduction process; Can access high-grade acid-dissolved titanium slag, by-product reductibility iron powder, and raw material be simple and easy to, low, the less investment of energy consumption, cost be low.
Low-temperature reduction of the present invention prepares the method for acid-dissolved titanium slag, is after ilmenite, carbon dust, sticker, yellow soda ash are mixed, and separates making the acid-dissolved titanium slag product through reduction, water-cooled, pulverizing, ferrotianium.
Described ilmenite, carbon dust, sticker, yellow soda ash mix according to mass ratio 10: 0.5~2: 0.5~2: 0.05~1.
Described sticker is a carboxy-propyl cellulose.
Described carboxy-propyl cellulose is carboxylic propyl methocel or carboxylic propyl group TKK 021.
Described reduction temperature is 600~800 ℃, and the recovery time is 1~2 hour.
Described water-cooled temperature is 10~30 ℃.
Fineness after the pulverizing is 200~300 orders.
Described ferrotianium is separated under 100~300 Gausses' the magneticstrength and carries out.
It is that acid-dissolved titanium slag is separated with iron powder that described ferrotianium separates.
The grade of described acid-dissolved titanium slag titanium oxide in one-level electromagnetism choosing raising acid-dissolved titanium slag.
Described acid-dissolved titanium slag is exactly that wherein the strongly magnetic mineral titanium slag is attracted to drum surface when ore pulp gets into field regions through the choosing of one-level electromagnetism; Weak magnetic and non magnetic ore are got rid of discharge; And the strongly magnetic mineral titanium slag that is adsorbed on the drum surface rotates with cylinder, is taken out of field regions, pours in the concentrate hopper with wash-down water; Accomplish separation operation, improve the grade of titanium oxide in the acid-dissolved titanium slag.
Described low-temperature reduction prepares the method for acid-dissolved titanium slag, specifically comprises the steps:
(1) ilmenite is mixed according to mass ratio 10: 0.5~2: 0.5~2: 0.05~1 with carbon dust, sticker, yellow soda ash, the cylindrical shell of packing into is put on the track of tunnel, with speed setting to 10~20cm/min, gets in the tunnel then and reduces; 600~800 ℃ of reduction temperatures, the recovery time in tunnel is 1~2 hour;
(2) to put into temperature rapidly be that 10~30 ℃ water cools off to the material after will reducing, and being crushed to fineness after the cooling is 200~300 orders;
(3) material after will pulverizing carries out the ferrotianium separation down of weak magnetic in magneticstrength is 100~300 Gausses' scope; What obtained by magnetic force absorption is the reductibility iron powder; Can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, improve the grade of titanium oxide in the acid-dissolved titanium slag.
The present invention is a kind of under the lower state of temperature, adopts the mode of tunnel to carry out reduced ilmenite, adopts the mode of water-cooled, pulverizing, ferrotianium separation, the choosing of one-level electromagnetism to obtain high-grade acid-dissolved titanium slag, the working method of by-product reductibility iron powder then.The principle of this method is under the lower state of temperature, and the iron with the high valence state in the ilmenite in reducing atmosphere is reduced to non-valent iron, iron is separated with titanium, thereby obtain high acid-dissolved titanium slag of titanium content and reductibility iron powder.
Employed raw material is simple and easy to, and carbon dust uses as reductive agent, can directly buy the commercially available prod or hard coal pulverized to get final product; Yellow soda ash is solubility promoter, directly buys the commercially available prod and gets final product; Sticker plays the effect that ilmenite, carbon dust, yellow soda ash are linked together, and is the commercially available prod.
Concrete process flow sheet of the present invention is as shown in Figure 1, and heat circulation synoptic diagram of the present invention is as shown in Figure 2.
The heat of water-cooled generating step among the present invention gets into another tunnel through induced draft fan, can recycle in the process of low-temperature reduction, has practiced thrift the energy.
Compared with prior art, beneficial effect of the present invention is:
(1) adopts low temperature that ilmenite is reduced, avoided traditional highly energy-consuming to carry out titanium and the isolating shortcoming of iron in the ilmenite, reduced energy consumption;
(2) mode of employing tunnel, the high facility investment of having avoided construction blast-furnace smelting and rotary hearth furnace to smelt;
(3) accomplish comprehensive utilization of resources, be back to use production to the heat in the reduction process, thereby reduced production cost.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is a heat circulation synoptic diagram of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe.
Ilmenite staple used among Comparative Examples of the present invention and the embodiment is as shown in table 1, and surplus is an impurity.
The present invention selects the carboxylic propyl methocel for use to used sticker among the embodiment.
The percentage composition (%) of table 1 ilmenite staple
Composition | TiO 2 | Ti 2O 3 | FeO | S | P | Ca | V 2O 5 | Fe 2O 3 | SiO 2 | AI 2O 3 |
Content | 46.05 | 0 | 22.61 | 0.10 | 0.15 | 0.52 | 0.11 | 15.0 | 11.2 | 4.23 |
Comparative Examples 1
The 200g ilmenite packed into to be lined with in the cylindrical shell of refractory brick, puts into airtight retort furnace, temperature is fixed in 1350 ℃ the scope, is slowly risen by low temperature, when temperature arrives 1350 ℃, is incubated 2 hours again, makes the iron in the ilmenite can fusion.Molten materials is poured out, obtained iron, the cooling of residue insolubles is blocky acid-dissolved titanium slag.Gained material TiO
2Be 69.3%, Ti
2O
3Be 12.6%, FeO is 16.9%, and S is 0.18%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 77.1%, TiO
2Be 15.5%, S is 0.16%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Embodiment 1
With 500g ilmenite and carbon dust, sticker, yellow soda ash according to mass ratio 10: 2: 1: after 0.05 ratio is mixed, behind the cylindrical shell of packing into, put on the track of tunnel, speed setting to 20cm/min, slowly got into tunnel; Temperature in the control tunnel remains on 800 ℃, reduces 1 hour; Material after the reduction is put into 20 ℃ of water and cool off rapidly, be crushed to fineness percent of pass in the 300 purpose scopes after the cooling and material carried out the ferrotianium separation greater than more than 90%.Control magnetic force carries out ferrotianium under magnetic a little less than 200 Gausses separates, and what obtained by magnetic force absorption is the reductibility iron powder, can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, obtain high-grade acid-dissolved titanium slag.Gained material TiO
2Be 72.9%, Ti
2O
3Be 11.7%, FeO is 9.42%, and S is 0.12%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 85.4%, TiO
2Be 8.5%, S is 0.09%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Embodiment 2
With 500g ilmenite and carbon dust, sticker, yellow soda ash according to mass ratio 10: 2: 1: after 0.075 ratio is mixed, behind the cylindrical shell of packing into, put on the track of tunnel, speed setting to 10cm/min, slowly got into tunnel; Temperature in the control tunnel remains on 600 ℃, reduces 1 hour; Material after the reduction is put into 20 ℃ of water cool off rapidly, being crushed to fineness after the cooling is 200 orders, and percent of pass carries out ferrotianium with material and separates greater than more than 95%.Control magnetic force carries out ferrotianium under magnetic a little less than 300 Gausses separates, and what obtained by magnetic force absorption is the reductibility iron powder, can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, obtain high-grade acid-dissolved titanium slag.Gained material TiO
2Be 72.3%, Ti
2O
3Be 13.2%, FeO is 8.32%, and S is 0.08%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 89.3%, TiO
2Be 5.5%, S is 0.06%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Embodiment 3
With 500g ilmenite and carbon dust, sticker, yellow soda ash according to mass ratio 10: 0.5: 1: after 0.1 ratio is mixed, behind the cylindrical shell of packing into, put on the track of tunnel, speed setting to 20cm/min, slowly got into tunnel; The temperature of control in the tunnel remains on 700 ℃, reductase 12 hour; Material after the reduction is put into 22 ℃ of water cool off rapidly, being crushed to fineness after the cooling is 300 orders, and percent of pass carries out ferrotianium with material and separates greater than more than 90%.Control magnetic force carries out ferrotianium under magnetic a little less than 300 Gausses separates, and what obtained by magnetic force absorption is the reductibility iron powder, can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, obtain high-grade acid-dissolved titanium slag.Gained material gains material TiO
2Be 74.2%, Ti
2O
3Be 12.6%, FeO is 10.3%, and S is 0.11%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 88.7%, TiO
2Be 7.8%, S is 0.09%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Embodiment 4
With 500g ilmenite and carbon dust, sticker, borax according to mass ratio 10: 1: 2: after 0.1 ratio is mixed, behind the cylindrical shell of packing into, put on the track of tunnel, speed setting to 20cm/min, slowly got into tunnel; Temperature in the control tunnel remains on 750 ℃, reduces 0.5 hour; Material after the reduction is put into 20 ℃ of water cool off rapidly, being crushed to fineness after the cooling is 300 orders, and percent of pass carries out ferrotianium with material and separates greater than more than 90%.Control magnetic force carries out ferrotianium under magnetic a little less than 100 Gausses separates, and what obtained by magnetic force absorption is the reductibility iron powder, can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, obtain high-grade acid-dissolved titanium slag.Gained material TiO
2Be 74.5%, Ti
2O
3Be 13.8%, FeO is 10.1%, and S is 0.05%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 86.9%, TiO
2Be 9.8%, S is 0.04%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Embodiment 5
With 500g ilmenite and carbon dust, sticker, yellow soda ash according to mass ratio 10: 1: 0.5: after 0.1 ratio is mixed, behind the cylindrical shell of packing into, put on the track of tunnel, speed setting to 15cm/min, slowly got into tunnel; Temperature in the control tunnel remains on 800 ℃, reduces 1 hour; Material after the reduction is put into 15 ℃ of water cool off rapidly, being crushed to fineness after the cooling is 300 orders, and percent of pass carries out ferrotianium with material and separates greater than more than 95%.Control magnetic force carries out ferrotianium under magnetic a little less than 100 Gausses separates, and what obtained by magnetic force absorption is the reductibility iron powder, can not by magnetic force absorption be acid-dissolved titanium slag, adopt the choosing of one-level electromagnetism again, obtain high-grade acid-dissolved titanium slag.Gained material TiO
2Be 77.1%, Ti
2O
3Be 11.9%, FeO is 10.7%, and S is 0.14%, and surplus is an impurity, National standard YB/T5285-2007 standard; Reductibility iron powder composition TFe is 87.5%, TiO
2Be 8.8%, S is 0.07%, and surplus is an impurity, satisfies the YB/T4170-2008 requirement.
Claims (10)
1. a low-temperature reduction prepares the method for acid-dissolved titanium slag, it is characterized in that it being after ilmenite, carbon dust, sticker, yellow soda ash are mixed, and separates making the acid-dissolved titanium slag product through reduction, water-cooled, pulverizing, ferrotianium.
2. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, it is characterized in that described ilmenite, carbon dust, sticker, yellow soda ash mix according to mass ratio 10: 0.5~2: 0.5~2: 0.05~1.
3. low-temperature reduction according to claim 1 and 2 prepares the method for acid-dissolved titanium slag, it is characterized in that described sticker is a carboxy-propyl cellulose.
4. low-temperature reduction according to claim 3 prepares the method for acid-dissolved titanium slag, it is characterized in that described carboxy-propyl cellulose is carboxylic propyl methocel or carboxylic propyl group TKK 021.
5. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, it is characterized in that described reduction temperature is 600~800 ℃, and the recovery time is 1~2 hour.
6. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, it is characterized in that described water-cooled temperature is 10~30 ℃.
7. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, and the fineness after it is characterized in that pulverizing is 200~300 orders.
8. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, it is characterized in that described ferrotianium is separated under 100~300 Gausses' the magneticstrength to carry out.
9. the method for preparing acid-dissolved titanium slag according to claim 1 or 8 described low-temperature reductions is characterized in that it is that acid-dissolved titanium slag is separated with iron powder that described ferrotianium separates.
10. low-temperature reduction according to claim 1 prepares the method for acid-dissolved titanium slag, it is characterized in that the grade of described acid-dissolved titanium slag titanium oxide in one-level electromagnetism choosing raising acid-dissolved titanium slag.
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Cited By (4)
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CN104150533A (en) * | 2014-08-08 | 2014-11-19 | 西南化工研究设计院有限公司 | Method for preparing anatase type titanium dioxide by acidolysis of clean titanium slag |
CN104178647A (en) * | 2014-09-02 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining grade of titanium slag smelted from titanium concentrate and method for smelting titanium slag from titanium concentrate |
CN107244694A (en) * | 2017-05-08 | 2017-10-13 | 朝阳金河粉末冶金材料有限公司 | The method that acid-dissolved titanium slag is produced using low-grade ilmenite |
CN109666805A (en) * | 2018-12-25 | 2019-04-23 | 海南文盛新材料科技股份有限公司 | A kind of ilmenite low-temperature reduction technique |
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CN104178647A (en) * | 2014-09-02 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining grade of titanium slag smelted from titanium concentrate and method for smelting titanium slag from titanium concentrate |
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CN107244694A (en) * | 2017-05-08 | 2017-10-13 | 朝阳金河粉末冶金材料有限公司 | The method that acid-dissolved titanium slag is produced using low-grade ilmenite |
CN109666805A (en) * | 2018-12-25 | 2019-04-23 | 海南文盛新材料科技股份有限公司 | A kind of ilmenite low-temperature reduction technique |
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Application publication date: 20120704 |