CN101298642B - Method for preparing titanium-aluminum-silicon alloy by carbothermal reduction method - Google Patents
Method for preparing titanium-aluminum-silicon alloy by carbothermal reduction method Download PDFInfo
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- CN101298642B CN101298642B CN2008100118629A CN200810011862A CN101298642B CN 101298642 B CN101298642 B CN 101298642B CN 2008100118629 A CN2008100118629 A CN 2008100118629A CN 200810011862 A CN200810011862 A CN 200810011862A CN 101298642 B CN101298642 B CN 101298642B
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- titaniferous
- silumin
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Abstract
The invention relates to a method for preparing an alloy of titanium, silicon and aluminum by using the carbothermy reduction method, and is characterized in that titaniferous slag, titaniferous ore or mixture of the titaniferous slag and the titaniferous ore are taken as raw titaniferous materials, and a carbonaceous reducing agent is added for mixing and milling; a caking agent is added for mixing, and titaniferous pellets are prepared and parched; the titaniferous pellets, silicon ore and the carbonaceous reducing agent are mixed according to a proportion that is required by a finished product so as to prepare charging materials; the prepared charging materials are placed into an ore-bearing electric arc furnace for smelting, thus obtaining the finished alloy product of titanium, silicon and aluminum. The method for preparing the alloy of titanium, silicon and aluminum by using the carbothermy reduction method uses titaniferous waste slag or gangue, adopts the carbothermy reduction method for directly preparing the alloy of titanium, silicon and aluminum in the ore-bearing electric arc furnace, thus lowering production cost and energy consumption, and having important meaning to the comprehensive utilization of the titaniferous slag and the titaniferous ore.
Description
Technical field
The invention belongs to material science, particularly a kind of method for preparing the titanium silumin with carbothermic method.
Background technology
Titanium sial multicomponent alloy is a kind of novel casting aluminum alloy, has good casting technique performance and high strength.The method of traditional mode of production titanium sial multicomponent alloy is to adopt fusion preparation casting to form, and just converts the method for mixing, and fine aluminium, pure titanium is melted earlier be made into aluminium titanium master alloy, again aluminium titanium and two master alloy remeltings of aluminium silicon is made into the titanium silumin.The pure metal that mix-melting method is required, their smeltings own just need the smelting technology process of a complexity, need to consume a large amount of energy.In order to produce fine aluminium, need technical process through complexity, consume huge energy, remove impurity such as silicon in the aluminium ore, titanium, make pure alumina, again fused salt electrolysis acquisition fine aluminium.Need remove aluminium silicon in the titanium mineral in order to produce pure titanium.When producing the titanium silumin, again by remelting several times.This method technical process is long, and complex process has been given up a large amount of valuable elements in Metal smelting and purification process, so the energy consumption height, cost is expensive, the investment cost height, and the construction period is long.
Panzhihua Region is being contained extremely abundant vanadium titano-magnetite, wherein contain titaniferous ores such as ilmenite and titanium spar, what present stage was at first utilized is ilmenite, Flos Bombacis Malabarici iron and steel group company exploitation vanadium titano-magnetite is a raw material, produce iron and steel and vanadium product, annual recyclable 500,000 tons contain titanium ore from the mine tailing of ore dressing.In addition, every year is also discharged about 3,000,000 tons titanium-containing blast furnace slag by Flos Bombacis Malabarici iron and steel group company, totally discharges more than 5,000 ten thousand tons so far, has not only wasted valuable titanium resource, but also serious environment pollution.
Present national natural mineral resource worsening shortages, cost of material rises steadily, and by produce the titanium silumin from blast furnace titaniferous slag and ilmenite concentrate, can economize on resources, and reduces environmental pollution, reduces the price of titanium silumin.The research of this respect is also fewer at present.
Summary of the invention
Problem at existing titanium silumin production aspect the invention provides a kind of method for preparing the titanium silumin with carbothermic method.Utilize titaniferous materials in the thermic arc stove of ore deposit, to be smelted directly into to contain the titanium silumin, titanium Alsimin of aluminium 20～60%, siliceous 30～60%, titaniferous 5～40% and be other alloy of base with the titanium sial.
Technical scheme of the present invention is:
1, be titaniferous materials with titanium-contained slag, the mixture that contains titanium ore or titanium-contained slag and contain titanium ore, with coke and charcoal is carbonaceous reducing agent, titaniferous materials and carbonaceous reducing agent are mixed, and selecting blending ratio according to the finished product needs is titaniferous materials: coke: charcoal=5～14: 2～3: 1; Adopt ball mill to wear into the powder of granularity then less than 1mm.
2, will grind good powder and add binding agent, and put into mixer mixing 4h, binding agent is a spent pulping liquor, add-on be binding agent account for whole material total masses 10%; Then with briquetting machine at pressure greater than being pressed into the titaniferous pelletizing that sphere diameter is 30～50mm under the 17MPa, put into the drying machine drying and dewatering then, require the moisture in the pelletizing to be no more than 1%.
3, titaniferous pelletizing, silica, coke, the charcoal after will drying pressed the required mixed preparation of finished product batch of material, with the batch of material for preparing join exchange or the DC-ore-heating electric arc furnace in carry out reduction reaction, smelting process is an arc-covering slag operation, operating voltage is 35V, electric current is 1500A, prepare the titanium silumin, wherein the contained total carbon of each composition is 0.8～1.0 times that complete chemical reaction theory needs the carbon amount; The equation of main chemical reactions is in the thermic arc stove of ore deposit:
Al
2O
3+3C＝2Al+3CO↑
SiO
2+2C＝Si+2CO↑
TiO
2+2C＝Ti+2CO↑
4, from the iron mouth of ore deposit thermic arc stove, emit titanium silumin liquid every 2～4 hours, obtain titanium silumin finished product.
Titanium-contained slag among the present invention is meant ferrotianium slag, blast furnace titaniferous slag etc., contains titanium ore and is meant titaniferous mine tailing (iron selection tailings, comprehensive mine tailing, select the titanium mine tailing), rutile, anatase octahedrite, ilmenite, titanium spar etc.
Carbonaceous reducing agent among the present invention is coke and charcoal, contains fixed carbon in the coke more than 81%; Contain fixed carbon in the charcoal more than 77%.
Titanium silumin finished product among the present invention is adjustable as required and contains aluminium 20～60%, and is siliceous 30～60%, the titanium silumin of titaniferous 5～40%, titanium Alsimin and be other alloy of base with the titanium sial.
The present invention prepares the method for titanium silumin with carbothermic method, make full use of reluctant titanium-contained slag of China and titaniferous mine tailing, valuable metals such as the titanium in the material, aluminium and silicon are recycled by producing the titanium silumin, turn waste into wealth, realize the comprehensive reutilization of resource, reduced environmental pollution.The present invention is directly by waste residue or mine tailing, adopt carbothermic method in the thermic arc stove of ore deposit directly from titaniferous, contain and produce the titanium silumin the aluminium thing, raw materials cost is low, simplified workflow, preparation process is simple, save energy, fixed investment is few, has reduced production cost and energy consumption; Carbothermic method of the present invention is the solid reaction of carrying out in the thermic arc stove of ore deposit, and utilization rate of electrical can reach 80%, and this is that other method is unapproachable.
Of the present inventionly prepare the method for titanium silumin with carbothermic method, the alloying constituent of preparation is controlled easily, by adjusting titanium-contained slag, containing the proportioning of titanium ore and silica, just can prepare the titanium silumin of heterogeneity content.The present invention has great importance to fully utilizing titanium-contained slag and containing titanium ore.
Embodiment
The invention process is selected the titanium-contained slag that discharges in the Flos Bombacis Malabarici iron and steel group company production process for use and is contained titanium ore as titaniferous materials, and its chemical ingredients is as shown in table 1.
Table 1 titanium-contained slag and the chemical ingredients wt% that contains titanium ore
| Chemical ingredients | TiO 2 | SiO 2 | Al 2O 3 | CaO | MgO | TFe |
| The ferrotianium slag | 13～18 | 0.1～1.0 | 60～75 | 8～11 | 0.5～14 | 0.5～2 |
| Blast furnace titaniferous slag | 21～25 | 17～24 | 13～15 | 20～28 | 7～9 | 2～8 |
| Iron selection tailings | 8～12 | 34～38 | 8～12 | 10～14 | 8～11 | 11～15 |
| Comprehensive mine tailing | 8～12 | 33～36 | 10～14 | 8～11 | 7～11 | 12～16 |
| Select the titanium mine tailing | 1～5 | 44～48 | 10～13 | 14～18 | 8～11 | 5～9 |
The main component mass percentage content is in the silica that the invention process adopts: SiO
2〉=98%.
Contain fixed carbon more than 81% in the coke that the invention process adopts; Contain fixed carbon in the charcoal more than 77%.
The spent pulping liquor that the invention process adopts is paper mill discharging spent pulping liquor.
Embodiment 1:
The employing titanium-contained slag is a raw material, and its main component mass percentage content is TiO
222%, SiO
223%, Al
2O
313%.
To wear into the powder of granularity less than 1mm after titanium-contained slag and the carbonaceous reducing agent mixing, its mixing quality ratio is a titanium-contained slag: coke: charcoal=14: 3: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material being put into the pair roller type pelletizer, is 30～50mm degree titaniferous pelletizing to be pressed into sphere diameter greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for material total mass 80%, silica accounts for material total mass 15%, and coke accounts for 4% of material total mass, and charcoal accounts for 1% of material total mass; Emitted the titanium silumin one time in 2 hours at interval, the titanium silumin composition of acquisition is a titanium 40%, silicon 38%, and aluminium 20%, surplus is Fe.
Embodiment 2:
The employing titanium-contained slag is a raw material, and its main component mass percentage content is TiO
213%, Al
2O
375%.
To wear into the powder of granularity less than 1mm after titanium-contained slag and the carbonaceous reducing agent mixing, its mixing quality ratio is a titanium-contained slag: coke: charcoal=5: 3: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material is put into the pair roller type pelletizer, to be pressed into the titaniferous pelletizing that sphere diameter is 30～50mm greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for total mass 50%, silica accounts for material total mass 35%, and coke accounts for 10% of material total mass, and charcoal accounts for 5% of material total mass; Emitted the titanium silumin one time in 3 hours at interval, the titanium silumin composition of acquisition is a titanium 14%, silicon 44%, and aluminium 40%, surplus is Fe.
Embodiment 3:
With the compound that contains titanium ore and titanium-contained slag is mixing raw material, and the main component mass percentage content that wherein contains titanium ore is TiO
212%, SiO
235%, Al
2O
313%, the main component mass percentage content of titanium-contained slag is TiO
218%, Al
2O
36O%.
To wear into the powder of granularity less than 1mm after mixing raw material and the carbonaceous reducing agent mixing, its mixing quality ratio is for containing titanium ore: titanium-contained slag: coke: charcoal=3: 3: 2: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material is put into the pair roller type pelletizer, to be pressed into the titaniferous pelletizing that sphere diameter is 30～50mm greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for material total mass 78%, silica accounts for material total mass 15%, and coke accounts for 5% of material total mass, and charcoal accounts for 2% of material total mass; Emitted the titanium silumin one time in 4 hours at interval, the titanium silumin composition of acquisition is a titanium 30%, silicon 30%, and aluminium 39%, surplus is Fe.
Embodiment 4:
The employing titanium-contained slag is a raw material, and its main component mass percentage content is TiO
216%, Al
2O
370%.
To wear into the powder of granularity less than 1mm after titanium-contained slag and the carbonaceous reducing agent mixing, its mixing quality ratio is a titanium-contained slag: coke: charcoal=6: 2: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material is put into the pair roller type pelletizer, to be pressed into the titaniferous pelletizing that sphere diameter is 30～50mm greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for total mass 50%, silica accounts for material total mass 35%, and coke accounts for 10% of material total mass, and charcoal accounts for 5% of material total mass; Emitted the titanium silumin one time in 3 hours at interval, the titanium silumin composition of acquisition is a titanium 5%, silicon 34%, and aluminium 60%, surplus is Fe.
Embodiment 5:
It is raw material that employing contains titanium ore, and its main component mass percentage content is TiO
212%, SiO
236%, Al
2O
310%.
To contain and wear into the powder of granularity less than 1mm after titanium ore and carbonaceous reducing agent mix, its mixing quality ratio is for containing titanium ore: coke: charcoal=13: 3: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material is put into the pair roller type pelletizer, to be pressed into the titaniferous pelletizing that sphere diameter is 30～50mm greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for material total mass 65%, silica accounts for material total mass 30%, and coke accounts for 4% of material total mass, and charcoal accounts for 1% of material total mass; Emitted the titanium silumin one time in 2 hours at interval, the titanium silumin composition of acquisition is a titanium 15%, silicon 60%, and aluminium 24%, surplus is Fe.
Embodiment 6:
It is raw material that employing contains titanium ore, and its main component mass percentage content is TiO
25%, SiO
244%, Al
2O
313%.
To contain and wear into the powder of granularity less than 1mm after titanium ore and carbonaceous reducing agent mix, its mixing quality ratio is for containing titanium ore: coke: charcoal=8: 3: 1; Add binding agent spent pulping liquor then in powder, put into the mixing machine thorough mixing, wherein the spent pulping liquor add-on is 10% of a material total mass; After mixing material is put into the pair roller type pelletizer, to be pressed into the titaniferous pelletizing that sphere diameter is 30～50mm greater than 17MPa pressure; The titaniferous pelletizing that obtains is put into the drying machine drying and dewatering, and the titaniferous pelletizing moisture content after the dehydration is less than 1%.
With the titaniferous pelletizing after the dehydration, silica, coke and charcoal are put into 63KVA ore deposit thermic arc stove and are smelted, smelting process is an arc-covering slag operation, and operating voltage is 35V, and electric current is 1500A, wherein the titaniferous pelletizing accounts for material total mass 80%, silica accounts for material total mass 15%, and coke accounts for 4% of material total mass, and charcoal accounts for 1% of material total mass; Emitted the titanium silumin one time in 2 hours at interval, the titanium silumin composition of acquisition is a titanium 6%, silicon 60%, and aluminium 33%, surplus is Fe.
Claims (5)
1. method for preparing the titanium silumin with carbothermic method, it is characterized in that may further comprise the steps: (1) with titanium-contained slag, contain titanium ore or both mixtures are titaniferous materials, coke and charcoal are carbonaceous reducing agent, titaniferous materials and carbonaceous reducing agent are mixed, and blending ratio is a titaniferous materials: coke: charcoal=5～14: 2～3: 1; Wear into the powder of granularity less than 1mm; (2) will grind good powder and add binding agent, the add-on of binding agent accounts for 10% of material total mass; Mix then, being pressed into sphere diameter under the condition of pressure greater than 17Mpa is the titaniferous pelletizing of 30～50mm, drying and dewatering then, and the moisture in the pelletizing is no more than 1%; (3) titaniferous pelletizing, silica, coke, charcoal are prepared batch of material in the required ratio of finished product, place Reaktionsofen to carry out reduction reaction the batch of material for preparing, came out of the stove, smelt the titanium silumin every 2～4 hours; Described titanium-contained slag is meant ferrotianium slag, blast furnace titaniferous slag, and wherein the chemical component weight per-cent of ferrotianium slag is TiO
213～18%, SiO
20.1～1.0%, Al
2O
360～75%, CaO 8～11%, and MgO 0.5～14%, and TFe 0.5～2%, and the chemical component weight per-cent of blast furnace titaniferous slag is TiO
221～25%, SiO
217～24%, Al
2O
313～15%, CaO 20～28%, and MgO 7～9%, and TFe 2～8%; The described titanium ore that contains is meant the titaniferous mine tailing, and the titaniferous mine tailing is iron selection tailings, comprehensive mine tailing, selects the titanium mine tailing, and the chemical component weight per-cent of iron selection tailings is TiO
28～12%, SiO
234～38%, Al
2O
38～12%, CaO 10～14%, and MgO 8～11%, and TFe 11～15%, and the weight percent of comprehensive mine tailing chemical ingredients is TiO
28～12%, SiO
233～36%, Al
2O
310～14%, CaO 8～11%, and MgO 7～11%, and TFe 12～16%, and the chemical component weight per-cent that selects the titanium mine tailing is TiO
21～5%, SiO
244～48%, Al
2O
310～13%, CaO 14～18%, and MgO 8～11%, and TFe 5～9%; Described binding agent is a spent pulping liquor.
2. method of producing the titanium silumin with carbothermic method according to claim 1 is characterized in that described Reaktionsofen and operation thereof: the Reaktionsofen of use is direct current or exchanges ore deposit thermic arc stove that smelting process is an arc-covering slag operation.
3. method of producing the titanium silumin with carbothermic method according to claim 1, it is characterized in that described preparation batch of material: titaniferous pelletizing, silica, coke and charcoal preparation batch of material are to adopt to lose the carbon prescription, and the contained total carbon of its each composition is 0.8～1.0 times that complete chemical reaction theory needs the carbon amount.
4. method of producing the titanium silumin with carbothermic method according to claim 1, it is characterized in that described titanium silumin finished product: produce in the thermic arc stove of ore deposit with carbothermic method and contain aluminium 20～60%, siliceous 30～60%, the titanium silumin of titaniferous 5～40%.
5. method of producing the titanium silumin according to claim 1 with carbothermic method, it is characterized in that described carbonaceous reducing agent: carbonaceous reducing agent is coke, charcoal, contains fixed carbon in the coke more than 81%; Contain fixed carbon in the charcoal more than 77%.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103243228B (en) * | 2013-06-03 | 2015-07-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing aluminum silicon titanium alloy with high-titanium blast furnace slag and fly ash as raw materials |
| CN103266232B (en) * | 2013-06-03 | 2015-07-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of aluminum-silicon-titanium alloy |
| CN103498091B (en) * | 2013-09-27 | 2015-11-25 | 包头稀土研究院 | The preparation method of niobium ferro-titanium and niobium ferro-titanium |
| CN103526027B (en) * | 2013-09-27 | 2016-02-03 | 包头稀土研究院 | Method and the niobium ferro-titanium of niobium ferro-titanium are prepared in profit reduction with carbon |
| NO20141486A1 (en) * | 2014-12-09 | 2016-06-10 | Elkem As | Energy efficient integrated process for the production of metals or alloys |
| CN105567970A (en) * | 2016-01-05 | 2016-05-11 | 北京科技大学 | Titanium carbide prepared by adopting ilmenite and smelting process and application of titanium carbide |
| CN106834891A (en) * | 2017-02-14 | 2017-06-13 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN106834880B (en) * | 2017-02-14 | 2019-01-18 | 东北大学 | A kind of preparation method of ferro-titanium |
| CN107385133A (en) * | 2017-07-24 | 2017-11-24 | 江苏省冶金设计院有限公司 | A kind of smelting process of v-ti magnetite concentrate |
| CN109457114B (en) * | 2018-11-08 | 2020-07-10 | 昆明理工大学 | Method for preparing titanium, silicon and titanium-silicon alloy by using titanium-containing slag |
| CN110563482B (en) * | 2019-10-17 | 2021-10-19 | 北京交通大学 | Method for preparing iron tailing porous ceramic through foaming, injection-coagulation forming and carbon thermal reduction reaction sintering |
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| US4917739A (en) * | 1984-08-10 | 1990-04-17 | Allied-Signal Inc. | Rapidly solidified aluminum-transition metal-silicon alloys |
| CN1257131A (en) * | 1998-12-16 | 2000-06-21 | 东北大学 | Technology for producing rare earth barium silicide alloy by carbon thermal reduction method |
| EP1546419B1 (en) * | 2002-08-29 | 2007-05-30 | Elkem AS | Production of metals and alloys using solid carbon produced from carbon-containing gas |
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2008
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|---|---|---|---|---|
| US4917739A (en) * | 1984-08-10 | 1990-04-17 | Allied-Signal Inc. | Rapidly solidified aluminum-transition metal-silicon alloys |
| CN1257131A (en) * | 1998-12-16 | 2000-06-21 | 东北大学 | Technology for producing rare earth barium silicide alloy by carbon thermal reduction method |
| EP1546419B1 (en) * | 2002-08-29 | 2007-05-30 | Elkem AS | Production of metals and alloys using solid carbon produced from carbon-containing gas |
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