CN106498108A - DRI and nitrogen are produced with titanomagnetite concentrate(Carbon)The method for changing titanium - Google Patents
DRI and nitrogen are produced with titanomagnetite concentrate(Carbon)The method for changing titanium Download PDFInfo
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- CN106498108A CN106498108A CN201610871280.2A CN201610871280A CN106498108A CN 106498108 A CN106498108 A CN 106498108A CN 201610871280 A CN201610871280 A CN 201610871280A CN 106498108 A CN106498108 A CN 106498108A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
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Abstract
The present invention provides a kind of titanomagnetite concentrate and produces the method that DRI and nitrogen (carbon) change titanium, belongs to technical field of resource utilization.After the method is by titanomagnetite concentrate, carbonaceous reducing agent, additive and binding agent mixed pelletizing or pressure ball, the roasted product that main component changes titanium for DRI and nitrogen (carbon) is obtained in 1200~1500 DEG C of reduction roastings, direct-reduction two products of iron product and Ti-enriched slag are sub-elected after roasted product ore grinding, and Ti-enriched slag obtains High Purity Nitrogen (carbon) through acidleach again and changes titanium products.This technique achieves the green composite to valuable component in titanomagnetite and utilizes, have the advantages that raw material sources extensive, flow process is short, low cost, added value of product are high.Finally give the nitrogen (carbon) of direct-reduction iron product of the iron recovery more than 90%, Iron grade more than 90% and the response rate more than 90%, purity more than 99% and change titanium products.
Description
Technical field
The present invention relates to technical field of resource utilization, particularly relate to one kind titanomagnetite concentrate production DRI and
The method that nitrogen (carbon) changes titanium.
Background technology
Titanomagnetite is a kind of important iron ore resource, but the smelting of titanomagnetite concentrate is world-famous puzzle, and China passes through
Cross the research of technique of decades, it is achieved that technological break-through, currently form the titanomagnetite industry of " blast furnace ironmaking-pneumatic steelmaking "
Production procedure.But the technique is produced as dominating with iron and steel, and titanium is enriched in blast furnace slag, but because of TiO2Content low (less than 25%),
Thing is mutually complicated, and the technique that there is presently no maturation can be processed, and therefore greatly wastes the titanium resource of preciousness.Additionally, a large amount of
Blast furnace titaniferous slag store up, occupy substantial amounts of soil, while also result in water and soil pollution problem.Therefore it is badly in need of exploitation clean and effective
New technology improve titanomagnetite in titanium utilization rate.
Nitrogen (carbon) is changed titanium and has that fusing point is high, hardness is big, chemical stability is good and metal moistening is little, conductive and superconductivity
The features such as performance is good, nontoxic, be widely used in machining, cosmetic decoration, Aero-Space and war industry, electronics and battery and
The various fields such as medical apparatus and instruments.At present, nitrogen (carbon) is changed titanium and is mainly with high-purity Ti O2Or ilmenite is raw material, using carbon nitridation also
Prepared by former technique, carbon reduction-nitridation is needed with high-purity Ti O2Or ilmenite is raw material.Further, it is also possible to directly former in material surface
Titanium film is changed in position synthetic nitrogen (carbon), and it is physical vaporous deposition and chemical gaseous phase that the most frequently used nitrogen (carbon) changes titanium film synthetic method
Sedimentation.Both of which is that pure titanium distils, and reacts with nitrogen in high-energy vacuum environment.Also can at high temperature, by
The gaseous mixture of titanium tetrachloride-nitrogen obtains nitrogen (carbon) with the mixing solid/liquid/gas reactions of ammonia-hydrogen and changes titanium, or titanium-hydrogen-nitrogen mixed gas are heated
To high temperature by graphite, formation film on matrix material after cooling, is deposited on.Either physical vaporous deposition or chemical gaseous phase
Sedimentation is both needed to pure titanium as raw material, and synthesis condition is harsh, and therefore production cost is high.
In view of the difficulty that reclaims titanium products from titanomagnetite blast furnace process titanium slag is big, high cost, environmental pollution are big, grind
Personnel are studied carefully with titanomagnetite and coal as raw material, using hot carbon reducing process synthesis Fe-TiC (N) composite, but such material
Impurity content is high-leveled and difficult with application.
Content of the invention
The technical problem to be solved in the present invention is to provide one kind titanomagnetite concentrate production DRI and nitrogen (carbon)
The method for changing titanium.
The method specifically includes following steps:
(1) pelletizing:By titanomagnetite concentrate, carbonaceous reducing agent, additive and binding agent, mixing and water adding is made by a certain percentage
Ball or pressure ball;
(2) reduction roasting:After step (1) gained carbonaceous pelletizing is dried, reduce at 1200~1500 DEG C of sintering temperature
Roasting generates the roasted product for changing titanium comprising DRI and nitrogen (carbon);The roasting of carbonaceous pelletizing is protected in reducing atmosphere or nitrogen
Carry out under shield, nitrogen atmosphere is conducive to nitrogen (carbon) to change titanium synthesis;Additive is added to have the effect that:A) promote iron mineral reduction
And nitrogen (carbon) changes the synthesis of titanium;D) metallic iron, nitrogen (carbon) is promoted to change growing up for titanium granule;C) gangue content is converted into readily soluble
In the material of acid, it is easy to the purification of subsequent nitridation carbon.
(3) ore grinding sorting:The roasted product of gained in step (2) is carried out ore grinding, then by low intensity magnetic separation or screening or
Person's low intensity magnetic separation-screening process integration obtains DRI and Ti-enriched slag;DRI is ferromagnetic substance, and granularity
Greatly, ductility is good, anti-wear performance is good, and other materials are weak magnetic or nonmagnetic, and general granularity is thinner, by low intensity magnetic separation or sieve
Divide or DRI can be separated with other materials by low intensity magnetic separation-screening process integration.Forming portion cyclotomy in roasted product
Screening after roasted ore simple crushing or ore grinding can be selected this portioned product by shape high-purity metallic iron coarse granule.Undersize is again
DRI and Ti-enriched slag are obtained through ore grinding, low intensity magnetic separation operation.
(4) acidleach purification:Gained Ti-enriched slag in step (3) is obtained High Purity Nitrogen (carbon) through the further remove impurity of acid solution and changes titanium
Product.The chemical property that nitrogen (carbon) changes titanium is extremely stable, insoluble in hydrochloric acid, sulphuric acid, phosphoric acid under room temperature, be slightly soluble in chloroazotic acid, nitric acid,
Fluohydric acid., therefore can be removed the impurity in Ti-enriched slag, obtain highly purified nitrogen (carbon) and change titanium products by acidleach.
Wherein, in step (1) titanium-containing magnet ore deposit concentrate used TFe grades>45%, TiO2Grade>5%.
In step (1) carbonaceous reducing agent be anthracite, bituminous coal, brown coal, graphite, coke, semicoke, petroleum coke, in biological Jiao
One or more combination;Additive be sodium carbonate, sodium sulfate, potassium carbonate, potassium sulfate, one or more group in sodium tetraborate
Close;In step (1), the mass ratio of titanium-containing magnet ore deposit concentrate, carbonaceous reducing agent, additive and binding agent is:100:(10~100):
(0~20):(0~10).
In step (2), roasted product is cooled down under air or nitrogen protection, or is burnt product through water quenching cooling.
In step (3), the grade of DRI is more than 90% more than the 90%, response rate.
In step (4) acidleach purification acid used for the one kind in hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid and perchloric acid or
Multiple combination.
The High Purity Nitrogen (carbon) obtained in step (4) is changed the purity of titanium valve body and is more than 99%, and titanium recovery rate is more than 90%.
The above-mentioned technical proposal of the present invention has the beneficial effect that:
In such scheme, directly by titanomagnetite production direct-reduction iron product and the high-purity titanium products of nitridation, with raw material
Wide material sources, flow process are short, value of the product is high and the characteristics of environmental friendliness, and green high-efficient make use of ferrum in titanomagnetite, titanium, vanadium
Resource.DRI and the response rate of the response rate more than 90%, Iron grade more than 90% are more than 99% more than 90%, purity
Nitrogen (carbon) changes titanium products.
Description of the drawings
Fig. 1 is the side that the use titanomagnetite concentrate production direct-reduction iron product and High Purity Nitrogen (carbon) of the present invention changes titanium products
Method flow chart.
Specific embodiment
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of titanomagnetite concentrate production direct-reduction iron product and High Purity Nitrogen (carbon) changes titanium products
Method, as shown in figure 1, including steps such as pelletizing, reduction roasting, ore grinding, sorting and acidleach, give with reference to specific embodiment
Explanation.
Embodiment 1
In certain titanomagnetite concentrate, grade is TFe 57.31%, TiO211.23%, wherein iron-bearing mineral is mainly titanium magnetic
Iron mine and a small amount of ilmenite, are substantially free of other gangue minerals.
By titanomagnetite concentrate:Anthracite:Waterglass in mass ratio 100:22:3 weigh mix homogeneously, then make in disk
Add water in ball machine generation carbonaceous pelletizing, carbonaceous pelletizing is dried at 105 DEG C, is then placed in graphite crucible, and is added a cover protection.Treat
When Muffle furnace is warming up to 1300 DEG C, graphite crucible is put into hearth roasting 90min, crucible is taken out at room temperature after terminating by roasting
Natural cooling.Ore grinding is carried out to pelletizing after roasting, mog accounts for 80% for -0.074, the ore pulp magnetic separation for obtaining, magnetic field are strong
Degree 100kA/m, magnetic concentrate are DRI, and Iron grade is 92.87%, and iron recovery is respectively 96.42%.Magnetic separation tail
Ore deposit is Ti-enriched slag, and Ti-enriched slag deionized water after hydrochloric acid, hydrofluoric acid dips stirring 24h is rinsed, and obtains high purity silicon nitride titanium valve body.
XRD and chemical analyses are carried out to the nitride powder for obtaining, its crystalline phase is TiN, and purity is 99.1%, and titanium recovery rate is
95%.
Embodiment 2
In certain titanomagnetite concentrate, grade is TFe 60.54%, TiO26.98%, wherein iron-bearing mineral is mainly titanium Magnet
Ore deposit and a small amount of ilmenite, are substantially free of other gangue minerals.
Titanomagnetite concentrate:Carbonaceous reducing agent:Additive:Binding agent in mass ratio 100:28:8:5 weigh mixing, then
The water for plus 12% is mixed.Carbonaceous reducing agent consists of anthracite:Bituminous coal:Activated carbon:Coke:Semicoke:Petroleum coke:The matter of graphite
Amount is than being 40:10:10:10:10:10:10, anthracite, bituminous coal, activated carbon, coke, semicoke, petroleum coke and graphite are industry
Product;Additive consists of calcium hydroxide:Potassium carbonate:Sodium sulfate:Sodium carbonate:Sodium sulfate:Calcium fluoride:Sodium borate mass ratio is
10:15:10:10:15:15:10, calcium hydroxide, potassium carbonate, potassium sulfate, sodium carbonate, sodium sulfate, calcium fluoride, sodium borate are work
Industry product;Binding agent consists of waterglass:Bentonite:Starch:Molasses:Sodium carboxymethyl cellulose mass ratio is 20:30:10:
30:10, waterglass, bentonite, starch, molasses, sodium carboxymethyl cellulose are industrial products.Mixed material is to roll-in ball
Carbonaceous pelletizing is generated in machine, carbonaceous pelletizing is dried at 105 DEG C, is then placed in graphite crucible, and is sealed.Treat Muffle furnace
When being warming up to 1330 DEG C, graphite crucible is put into hearth roasting 70min, crucible is taken out naturally cold at room temperature by roasting after terminating
But.Agglomerates are carried out with ore grinding, mog accounts for 80% for -0.4, and ore milling product is sieved using the sieve of 0.2mm,
Oversize is high-grade DRI, and Iron grade is 95.43%.Undersize is carried out ore grinding, mog again
92% is accounted for for -0.074, gained ore pulp carries out magnetic separation, magnetic field intensity is 70kA/m, and magnetic concentrate Iron grade is 91.01%, ferrum
Overall recovery is 96.32%.Ti-enriched slag is through persalt, sulphuric acid, phosphoric acid, nitric acid, Fluohydric acid., boric acid, perchloric acid and benzenedisulfonic acid
After mixed acid soaking and stirring 28h, deionized water is rinsed, and is obtained High Purity Nitrogen (carbon) and is changed titanium valve body, and nitrogen (carbon) is changed the purity of titanium and is
99.38%, titanium recovery rate is 92.33%.
Embodiment 3
In certain titanomagnetite concentrate, grade is TFe 47.87%, TiO219.01%, wherein iron-bearing mineral is mainly titanium magnetic
Iron mine and a small amount of ilmenite, are substantially free of other gangue minerals.
Titanomagnetite concentrate:Carbonaceous reducing agent:Additive:Binding agent in mass ratio 100:18:9:5 weigh mixing.Carbonaceous
Reducing agent consists of anthracite:Bituminous coal:Activated carbon:Coke:Semicoke:Petroleum coke:The mass ratio of graphite is 50:5:15:5:15:
5:5, anthracite, bituminous coal, activated carbon, coke, semicoke, petroleum coke and graphite are industrial products;Additive consists of hydroxide
Calcium:Potassium carbonate:Sodium sulfate:Sodium carbonate:Sodium sulfate:Calcium fluoride:Sodium borate mass ratio is 8:20:15:5:20:10:22, hydroxide
Calcium, potassium carbonate, potassium sulfate, sodium carbonate, sodium sulfate, calcium fluoride, sodium borate are industrial products;Binding agent consists of waterglass:
Bentonite:Starch:Molasses:Sodium carboxymethyl cellulose mass ratio is 20:30:10:30:10, waterglass, bentonite, starch, useless
Syrup, sodium carboxymethyl cellulose are industrial products.Mixed material adds water in disc balling machine generation carbonaceous pelletizing, by carbon containing
Pelletizing is dried at 105 DEG C, is then placed in graphite crucible, and is added a cover protection.When Muffle furnace is warming up to 1250 DEG C, by graphite earthenware
Crucible is put into hearth roasting 150min, and crucible is taken out natural cooling at room temperature after terminating by roasting.Ore grinding is carried out to agglomerates,
Mog accounts for 75% for -0.074, and the ore pulp for obtaining carries out magnetic separation, and magnetic field intensity is 140kA/m, and magnetic concentrate is straight
Reduced iron is connect, Iron grade is 93.02%, and iron recovery is respectively 97.13%.Ti-enriched slag through persalt, sulphuric acid, phosphoric acid, nitric acid,
After Fluohydric acid., boric acid, perchloric acid and benzenedisulfonic acid mixed acid soaking and stirring 35h, deionized water is rinsed repeatedly, and obtaining purity is
99.40% nitride powder, titanium recovery rate are 94.30%.
Embodiment 4
In certain titanomagnetite concentrate, grade is TFe 55.22%, TiO213.32%, wherein iron-bearing mineral is mainly titanium magnetic
Iron mine and a small amount of ilmenite, are substantially free of other gangue minerals.
Titanomagnetite concentrate:Carbonaceous reducing agent:Additive in mass ratio 100:35:20 weigh mixing.Carbonaceous reducing agent
Consist of anthracite:Bituminous coal:Activated carbon:Coke:Semicoke:Petroleum coke:The mass ratio of graphite is 50:5:15:5:15:5:5, smokelessly
Coal, bituminous coal, activated carbon, coke, semicoke, petroleum coke and graphite are industrial products;Additive consists of calcium hydroxide:Carbonic acid
Potassium:Sodium sulfate:Sodium carbonate:Sodium sulfate:Calcium fluoride:Sodium borate mass ratio is 25:15:7:10:13:15:15, calcium hydroxide, carbon
Sour potassium, potassium sulfate, sodium carbonate, sodium sulfate, calcium fluoride, sodium borate are industrial products;Mixed material adds in disc balling machine
Water generating carbonaceous pelletizing, carbonaceous pelletizing is dried at 105 DEG C, carbonaceous pelletizing is put in atmosphere furnace, and nitrogen charging gas shielded is warming up to
1460 DEG C, 40min is then incubated, roasting is cooled down under nitrogen protection with stove after terminating.Ore grinding, ore grinding are carried out to pelletizing after roasting
Fineness accounts for 60% for -0.074, and the ore pulp for obtaining carries out magnetic separation, and magnetic field intensity is 130kA/m, and magnetic concentrate is directly to be gone back
Former ferrum, Iron grade are 92.34%, and iron recovery is respectively 96.88%.Ti-enriched slag is through persalt, sulphuric acid, phosphoric acid, nitric acid, hydrogen fluorine
After acid, boric acid, perchloric acid and benzenedisulfonic acid mixed acid soaking and stirring 30h, deionized water is rinsed repeatedly, obtains High Purity Nitrogen (carbon)
Change titanium valve body.XRD and chemical analyses are carried out to the nitride powder for obtaining, its crystalline phase is TiCN, and purity is 99.38%, titanium
The response rate is 90.45%.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from principle of the present invention, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of titanomagnetite concentrate produces the method that DRI and nitrogen (carbon) change titanium, it is characterised in that:Including as follows
Step:
(1) pelletizing:Titanomagnetite concentrate, carbonaceous reducing agent, additive and binding agent are mixed by a certain percentage, is then added water and is made
Ball or pressure ball;
(2) reduction roasting:After step (1) gained carbonaceous pelletizing is dried, reduction roasting at 1200~1500 DEG C of sintering temperature
Generate the roasted product for changing titanium comprising DRI and nitrogen (carbon);
(3) ore grinding sorting:The roasted product of gained in step (2) is carried out ore grinding, then by low intensity magnetic separation or screening or weak
Magnetic separation-screening process integration obtains direct-reduction iron product and Ti-enriched slag;
(4) acidleach purification:Gained Ti-enriched slag in step (3) is obtained High Purity Nitrogen (carbon) by acidleach and changes titanium products.
2. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:The TFe grades of titanomagnetite concentrate used in step (1)>45%, TiO2Grade>5%.
3. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:In step (1), carbonaceous reducing agent is anthracite, bituminous coal, brown coal, graphite, coke, semicoke, petroleum coke, biological Jiao
In one or more combination.
4. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:In step (1), additive is sodium carbonate, sodium sulfate, potassium carbonate, potassium sulfate, the one kind or many in sodium tetraborate
Kind.
5. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:In step (2), the roasting of carbonaceous pelletizing is carried out under reducing atmosphere or nitrogen protection;In step (2), roasting is produced
Product are cooled down under air or nitrogen protection, or roasted product is through water quenching cooling.
6. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:In step (1), the mass ratio of titanomagnetite concentrate, carbonaceous reducing agent, additive and binding agent is:100:(10
~100):(0~20):(0~10).
7. the method that use titanomagnetite concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, which is special
Levy and be:In step (3), in ore grinding assorting room, ore grinding is dry grinding or wet grinding, and ore grinding number of times is no less than once;It is sieving through
Journey is dry screen or wet screening, and low intensity magnetic separation and screening number of times are no less than once;The magnetic field intensity of low intensity magnetic separation is 30~200KA/m.
8. the method that use titanium-containing magnet ore deposit concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, its
It is characterised by:In step (4) acidleach purification acid used be hydrochloric acid, in sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid, perchloric acid one
Plant or multiple.
9. the method that use titanium-containing magnet ore deposit concentrate production DRI according to claim 1 and nitrogen (carbon) change titanium, its
It is characterised by:The direct-reduction iron recovery for finally giving is more than 90% more than 90%, Iron grade;High Purity Nitrogen (carbon) changes titanium products
The response rate is more than 99% more than 90%, purity.
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CN115010170A (en) * | 2022-07-04 | 2022-09-06 | 重庆大学 | TiCl preparation by utilizing titanium-containing blast furnace slag 4 Method (2) |
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CN110002889A (en) * | 2019-05-20 | 2019-07-12 | 攀枝花学院 | A kind of Ti (C, N) base refractory material and the method for producing Ti (C, N) base refractory material using 50 titanium slags |
CN112024121A (en) * | 2020-08-31 | 2020-12-04 | 重庆优钛实业有限公司 | Vanadium titano-magnetite separation and extraction method |
CN115010170A (en) * | 2022-07-04 | 2022-09-06 | 重庆大学 | TiCl preparation by utilizing titanium-containing blast furnace slag 4 Method (2) |
CN115010170B (en) * | 2022-07-04 | 2023-09-22 | 重庆大学 | TiCl preparation by using titanium-containing blast furnace slag 4 Is a method of (2) |
CN115821140A (en) * | 2022-11-24 | 2023-03-21 | 河南融发新材料科技有限公司 | Titanium-containing alloy for metallurgy and low-cost production method thereof |
CN115821140B (en) * | 2022-11-24 | 2024-04-30 | 河南融发新材料科技有限公司 | Titanium-containing alloy for metallurgy and low-cost production method thereof |
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