CN108754144B - Production method of low-iron-content high-quality sponge titanium - Google Patents

Production method of low-iron-content high-quality sponge titanium Download PDF

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CN108754144B
CN108754144B CN201810898141.8A CN201810898141A CN108754144B CN 108754144 B CN108754144 B CN 108754144B CN 201810898141 A CN201810898141 A CN 201810898141A CN 108754144 B CN108754144 B CN 108754144B
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titanium
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CN108754144A (en
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盛卓
李开华
张敏
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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    • 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
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    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
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Abstract

The invention discloses a production method of sponge titanium with low iron content and high quality, belonging to the technical field of non-ferrous metal smelting. The invention aims to solve the technical problem that the content of Fe in titanium sponge prepared by the existing method is higher, and provides a production method of low-iron-content high-quality titanium sponge, which comprises the steps of selecting a specific reaction vessel reaction zone material, carrying out titanizing on the inner surfaces of a reaction vessel and a liquid magnesium vacuum ladle, avoiding pollution of reaction equipment to Fe impurities in the titanium sponge, limiting the transport temperature of liquid magnesium, refining the liquid magnesium to remove iron, enriching iron impurities introduced by the liquid magnesium to the bottom of a titanium lump, and separating materials at the bottom of the titanium lump to realize the production of the low-iron-content high-quality titanium sponge, wherein the iron content can be as low as 0.01% by weight.

Description

Production method of low-iron-content high-quality sponge titanium
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a production method of sponge titanium with high content of low iron and high quality.
Background
The titanium and the titanium alloy have the characteristics of low density, high strength, corrosion resistance, good biocompatibility and the like, and are widely applied to the fields of aerospace, deep sea titanium materials, biological materials and the like. The titanium sponge is used as an important raw material for preparing titanium and titanium alloy, and the impurity content of the titanium sponge determines the mechanical properties and the application field of the titanium and titanium alloy, for example, the Fe and Ni impurity content of Ti-24Al-20Nb-0.5Mo alloy influences the creep deformation and tensile property of the alloy; the Fe impurity content of pure titanium affects its high temperature formability.
Currently, titanium sponge is industrially produced only by magnesiothermic process, i.e. by charging TiCl into a reaction vessel containing liquid magnesium4The reduction reaction is allowed to occur on the inner surface of the reaction vessel intersecting the liquid magnesium. TiCl (titanium dioxide)4The magnesiothermic reduction reaction of (a) is a strongly exothermic process, and thus a large amount of reaction heat is released in the reaction zone. The reaction vessel used for producing the titanium sponge is mostly stainless steel or carbon steel, although before useThe inner surface of the titanium-plated layer is subjected to titanizing treatment by adopting physical vapor deposition and chemical vapor deposition, but the component of the titanizing layer is still Ti-Fe alloy, and the higher reaction temperature also promotes the dissolution of Fe atoms of the titanizing layer into liquid magnesium, so that the titanium sponge is polluted by iron impurities finally.
Magnesium and TiCl liquid for producing titanium sponge by magnesium thermal method4The raw material is Ti and Fe atoms with stronger attractive force than Mg and Fe atoms, so TiCl4FeCl in (1)3Iron impurities reduced by magnesium are enriched in the titanium sponge, impurities in the liquid magnesium are also enriched in the titanium sponge, and finally the titanium sponge is polluted by the iron impurities.
Disclosure of Invention
The invention aims to solve the technical problem that the sponge titanium prepared by the existing method has high Fe content and influences the performance of the sponge titanium.
The technical scheme adopted by the invention for solving the technical problems is to provide a production method of sponge titanium with low iron content and high quality, which comprises the following steps: A. preparing a reaction container: before the reaction vessel is used, carrying out titanizing treatment on the inner surface of the reaction vessel; the reaction vessel is divided into a reaction zone and a non-reaction zone; wherein the material of the reaction zone is a titanium steel composite plate, the surface material of the reaction zone is pure titanium, the outer surface material of the reaction zone is 1Cr18Ni9Ti stainless steel, the thickness of the pure titanium layer is 5-10 mm, and the thickness of the stainless steel layer is 20-25 mm; the material of the non-reaction zone is 1Cr18Ni9Ti stainless steel;
B. and (3) transporting liquid magnesium: carrying out titanizing treatment on the inner surface of the liquid magnesium vacuum ladle, transferring the liquid magnesium into a titanized reaction container by using the titanized liquid magnesium vacuum ladle, and controlling the extraction temperature of the liquid magnesium to be 670-690 ℃;
C. placing the titanized reaction container in a reduction electric furnace, adding liquid magnesium into the reaction container to enable the surface of the liquid magnesium to be within the height range of a reaction zone of the reaction container, then heating the liquid magnesium to 800-850 ℃, and adding TiCl into the reaction container4100～300Kg，TiCl4Adding the mixture at a speed of 100-150 Kg/h, keeping the temperature of 800-850 ℃ for 1-2 h, and continuously adding TiCl into the reaction vessel4，TiCl4Adding the mixture at a speed of 300-500 Kg/h, and then performing vacuum evaporation on the reduction productAnd (3) after distillation, separating the sponge titanium with the mass of 0.5-1.5% of the bottom of the sponge titanium after the sponge titanium is discharged from the furnace, and obtaining the sponge titanium with low iron content and high quality.
In the production method of the sponge titanium with low iron content and high quality, in the step A, the operation of titanizing the inner surface of the reaction vessel is as follows: adding industrial grade-1 sponge titanium into a reaction container, connecting the reactor with a vacuum system, vacuumizing the reaction container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuing for 30-60 hours, closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to 300 ℃, cooling to room temperature, and taking out the reaction container for later use.
In the production method of the sponge titanium with low iron content and high quality, when the reaction container is subjected to titanizing treatment, the addition amount of the industrial grade-1 sponge titanium is as follows: 100-300 Kg of titanium sponge is added into a reaction vessel with the volume of per cubic meter.
In the production method of the sponge titanium with the low iron content and the high quality, in the step B, the operation of the titanizing treatment on the inner surface of the liquid magnesium vacuum ladle is as follows: placing the two-man ladle in a titanizing container, adding industrial grade-1 sponge titanium into the titanizing container, connecting the titanizing container with a vacuum system, vacuumizing the titanizing container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuing for 30-60 hours, closing a temperature control system of the electric furnace, stopping the vacuum system when the temperature is reduced to 300 ℃, cooling to room temperature, and taking out the two-man ladle for later use.
In the production method of the sponge titanium with low iron content and high quality, when liquid magnesium vacuum ladle is used for coating, the addition amount of the industrial grade-1 sponge titanium is as follows: adding 100-300 Kg of titanium sponge into a titanizing container with the volume of per cubic meter.
In the production method of the sponge titanium with the low iron content and the high quality, in the step C, the adding amount of the liquid magnesium accounts for 70-80% of the volume of the reactor.
Wherein, in the step C of the production method of the sponge titanium with low iron content and high quality, the TiCl is added4The total addition amount of the magnesium liquid is 2.0 to up to one hundred percent of the addition mass of the magnesium liquid2.3 times.
Wherein, in the step C of the production method of the sponge titanium with high low iron content and high quality, the TiCl is added4Middle FeCl3The mass percentage content is 0.0003-0.0006%.
In the production method of the sponge titanium with low iron content and high quality, in the step C, the temperature of vacuum distillation is 980-1020 ℃, the vacuum degree is 0.1-10 Pa, and the time is 70-90 hours.
The invention has the beneficial effects that:
according to the method, firstly, the reaction zone of the reaction container is prepared by using the titanium steel composite plate, and meanwhile, the inner surface of the reaction container is subjected to titanizing by adopting a vacuum vapor deposition method, so that the pollution of the reaction container to the impurities of the titanium sponge Fe is effectively avoided; then titanizing the inner surface of the liquid magnesium vacuum ladle, limiting the transport temperature of the liquid magnesium, refining the liquid magnesium to remove iron, enriching iron impurities introduced by the liquid magnesium at the bottom of the titanium lump, separating materials at the bottom of the titanium lump to realize high-quality titanium sponge with low iron content, wherein the mass percentage content of iron in the obtained titanium sponge can be as low as 0.01%.
Drawings
FIG. 1 is a schematic view of a reaction vessel of the present invention.
Detailed Description
Specifically, the production method of the sponge titanium with low iron content and high quality comprises the following steps: A. preparing a reaction container: before the reaction vessel is used, carrying out titanizing treatment on the inner surface of the reaction vessel; the reaction vessel is divided into a reaction zone and a non-reaction zone; wherein the material of the reaction zone is a titanium steel composite plate, the surface material of the reaction zone is pure titanium, the outer surface material of the reaction zone is 1Cr18Ni9Ti stainless steel, the thickness of the pure titanium layer is 5-10 mm, and the thickness of the stainless steel layer is 20-25 mm; the material of the non-reaction zone is 1Cr18Ni9Ti stainless steel;
B. and (3) transporting liquid magnesium: carrying out titanizing treatment on the inner surface of the liquid magnesium vacuum ladle, transferring the liquid magnesium into a titanized reaction container by using the titanized liquid magnesium vacuum ladle, and controlling the extraction temperature of the liquid magnesium to be 670-690 ℃;
C. placing the titanized reaction vessel in a reduction electric furnace, and adding the titanium into the reaction vesselAdding liquid magnesium into the reaction container to ensure that the surface of the liquid magnesium is within the height range of a reaction zone of the reaction container, then heating the liquid magnesium to 800-850 ℃, and adding TiCl into the reaction container4100～300Kg，TiCl4Adding the mixture at a speed of 100-150 Kg/h, keeping the temperature of 800-850 ℃ for 1-2 h, and continuously adding TiCl into the reaction vessel4，TiCl4And (3) adding the titanium sponge into the reaction kettle at the speed of 300-500 Kg/h, then carrying out vacuum distillation on the reduction product, and after the distillation is finished, separating the titanium sponge with the mass of 0.5-1.5% of the bottom of the titanium sponge after the titanium sponge is discharged from the furnace to obtain the titanium sponge with low iron content and high quality.
The method divides the reaction vessel into a reaction zone and a non-reaction zone, and the inventor finds that the Fe impurity has three main sources in the production of the titanium sponge: reaction vessel, liquid magnesium and TiCl4The introduced amount of the reaction vessel is about 70 percent, and the iron impurities introduced by the reactor mainly come from the reaction zone, because the temperature of the reaction zone is higher and the iron is easier to diffuse into the liquid magnesium, the invention selects the specific reaction vessel material and carries out titanizing treatment on the reaction vessel.
In the method, the reaction zone of the reaction vessel is made of a titanium steel composite plate, the surface of the composite plate is made of pure titanium, the outer surface of the composite plate is made of 1Cr18Ni9Ti stainless steel, the thickness of the pure titanium layer is 5-10 mm, and the thickness of the stainless steel layer is 20-25 mm; the material of the non-reaction zone is 1Cr18Ni9Ti stainless steel, so that the introduction of Fe in the reaction vessel into the titanium sponge is avoided as much as possible, and the cost is saved. Meanwhile, carrying out titanizing treatment on the inner surface of the reaction vessel: adding industrial grade-1 sponge titanium into a reaction container, connecting the reactor with a vacuum system, vacuumizing the reaction container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuing for 30-60 hours, closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to 300 ℃, cooling to room temperature, and taking out the reaction container for later use. In order to ensure the titanizing effect, when the reaction vessel is subjected to titanizing treatment, the addition amount of the industrial grade-1 sponge titanium is as follows: 100-300 Kg of titanium sponge is added into a reaction vessel with the volume of per cubic meter.
In the method, the height of the added liquid magnesium is a reaction interface, the range of 1-2 m above and below the reaction interface is a reaction zone, and the rest parts are non-reaction zones; for example, the reactor height is about 4 meters, the liquid magnesium height is typically about 1 meter from the upper reactor flange, and the reaction zone is about 2 meters.
The method comprises the steps of firstly carrying out titanizing treatment on the inner surface of a liquid magnesium vacuum ladle, placing the ladle in a titanizing container, adding 1000 Kg-3000 Kg of industrial grade 1 titanium sponge into the titanizing container, connecting the titanizing container with a vacuum system, vacuumizing the titanizing container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuously coating for 30-60 hours, closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to below 300 ℃, cooling to the room temperature, and taking out the ladle. In order to ensure the titanizing effect, when the liquid magnesium vacuum ladle is subjected to titanizing treatment, the addition amount of the industrial grade-1 sponge titanium is as follows: adding 100-300 Kg of titanium sponge into a titanizing container with the volume of per cubic meter.
The liquid magnesium used in the method is low-iron-content liquid magnesium produced by magnesium electrolysis, the content of magnesium and iron in the electrolytic crude liquid is 0.015-0.025%, because the inner surface of the liquid magnesium vacuum ladle is subjected to titanizing treatment, a steel transfer container is prevented from being directly contacted with the liquid magnesium, and the iron content of the crude liquid magnesium is only increased by a very small amount, namely 0.20-0.030%, after the crude liquid magnesium is transferred into a reaction container. Meanwhile, the liquid magnesium transfer temperature is reduced, the liquid magnesium pumping temperature is controlled to be 670-690 ℃, and the reduction of the content of liquid magnesium Fe is facilitated; further using TiCl4Refining the liquid magnesium to remove iron, heating the liquid magnesium to 800-850 ℃, and adding TiCl into the reaction container4100～300Kg，TiCl4The adding speed is 100-150 Kg/h, and the temperature is kept at 800-850 ℃ for 1-2 h to refine and deironing the liquid magnesium, so that the generated titanium sponge adsorbs Fe impurities in the liquid magnesium, and the Fe impurities are finally enriched at the bottom of the titanium lump, so that the Fe content of the liquid magnesium is further reduced, and the preparation of the titanium sponge with low iron content is facilitated.
TiCl used in refining liquid magnesium4Is prepared by a molten salt chlorination method and is used for preparing crude TiCl4Rectifying and purifying to remove FeCl3、FeCl2And impurities are removed to obtainIs fine TiCl4FeCl of3The content is 0.0003 to 0.0006%.
Because the bonding force of Ti and Mg atoms is stronger than that of Mg and Fe, the liquid magnesium is put in a reaction container, heated and added with TiCl4The Fe impurity in Mg can be enriched at the bottom of the titanium lump, and after the titanium sponge is discharged from the furnace, the titanium sponge with the bottom accounting for 0.5-1.5% of the mass is separated, so that the high-quality titanium sponge with low iron content can be obtained.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
The reaction vessel for magnesiothermic reduction is manufactured according to the figure 1, the volume of the reaction vessel is 10 cubic meters, the material of the reaction zone is a titanium steel composite plate, the material of the surface of the reaction vessel is pure titanium, the material of the outer surface of the reaction vessel is 1Cr18Ni9Ti stainless steel, the thickness of the pure titanium layer is 5mm, and the thickness of the stainless steel layer is 25 mm; the material of the non-reaction zone is 1Cr18Ni9Ti, and the thickness is 30 mm; the reaction zone and the non-reaction zone of the reaction vessel are connected by welding;
before the reaction vessel is used, carrying out titanizing treatment on the inner surface of the reaction vessel, firstly adding 1000Kg of industrial grade 1 sponge titanium (GB/T2524-2010) into the reaction vessel, connecting the titanizing vessel with a vacuum system, vacuumizing the titanizing vessel, starting an electric furnace when the vacuum degree of the titanizing vessel reaches 1Pa, controlling the temperature to be 1000 ℃, continuously coating for 30 hours, then closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to be below 300 ℃, and taking out the reaction vessel for later use after the reaction vessel is cooled to room temperature;
carrying out titanizing treatment on the inner surface of a liquid magnesium vacuum ladle, firstly placing the ladle in a titanizing container, adding 1000Kg of industrial grade 1 titanium sponge (GB/T2524-2010) into the titanizing container, connecting the titanizing container with a vacuum system, vacuumizing the titanizing container, starting an electric furnace when the vacuum degree of the titanizing container reaches 1Pa, controlling the temperature to be 1000 ℃, continuously coating for 30 hours, then closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to be below 300 ℃, and taking out the ladle for later use when the temperature is reduced to room temperature;
using titanized liquid magnesium ladle to transfer liquid magnesium and pumping liquid magnesiumThe temperature is 690 ℃, then the magnesium is transferred into the reaction vessel, the surface of the liquid magnesium is in the height range of the reaction zone of the reaction vessel, then the temperature of the liquid magnesium is raised to 850 ℃, TiCl is added into the reaction vessel4300Kg，TiCl4Adding the magnesium powder at the speed of 150Kg/h, and then keeping the temperature at 850 ℃ for 2h to refine and remove iron in the liquid magnesium; then, TiCl was continuously added to the reaction vessel4，TiCl4The adding speed is 400Kg/h, the reduced product is subjected to vacuum distillation after the preset adding amount is reached, the sponge titanium with the bottom of 1 percent of the mass is separated after the sponge titanium is discharged from the furnace, and the iron mass content in the finally obtained sponge titanium is 0.010 percent.

Claims (10)

1. The production method of the sponge titanium with low iron content and high quality is characterized in that: the method comprises the following steps:
A. preparing a reaction container: before the reaction vessel is used, carrying out titanizing treatment on the inner surface of the reaction vessel; the reaction vessel is divided into a reaction zone and a non-reaction zone; wherein the material of the reaction zone is a titanium steel composite plate, the material of the inner surface of the reaction zone is pure titanium, the material of the outer surface of the reaction zone is 1Cr18Ni9Ti stainless steel, the thickness of the pure titanium layer is 5-10 mm, and the thickness of the stainless steel layer is 20-25 mm; the material of the non-reaction zone is 1Cr18Ni9Ti stainless steel;
B. and (3) transporting liquid magnesium: carrying out titanizing treatment on the inner surface of the liquid magnesium vacuum ladle, transferring the liquid magnesium into a titanized reaction container by using the titanized liquid magnesium vacuum ladle, and controlling the extraction temperature of the liquid magnesium to be 670-690 ℃;
C. placing the titanized reaction container in a reduction electric furnace, adding liquid magnesium into the reaction container to enable the surface of the liquid magnesium to be within the height range of a reaction zone of the reaction container, then heating the liquid magnesium to 800-850 ℃, and adding TiCl into the reaction container4100~300Kg，TiCl4Adding the mixture at a speed of 100-150 Kg/h, keeping the temperature of 800-850 ℃ for 1-2 h, and continuously adding TiCl into the reaction vessel4，TiCl4And (3) adding the titanium sponge into the reaction kettle at the speed of 300-500 Kg/h, then carrying out vacuum distillation on the reduction product, and after the distillation is finished, separating the titanium sponge with the mass of 0.5-1.5% of the bottom of the titanium sponge after the titanium sponge is discharged from the furnace to obtain the titanium sponge with low iron content and high quality.
2. The method for producing titanium sponge with low iron content and high quality as claimed in claim 1, wherein: in the step A, the operation of titanizing the inner surface of the reaction vessel comprises the following steps: adding industrial grade-1 sponge titanium into a reaction container, connecting the reactor with a vacuum system, vacuumizing the reaction container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuing for 30-60 hours, closing a temperature control system of the electric furnace, closing the vacuum system when the temperature is reduced to 300 ℃, cooling to room temperature, and taking out the reaction container for later use.
3. The method for producing titanium sponge with low iron content and high quality as claimed in claim 2, wherein: when the reaction vessel is subjected to titanizing treatment, the addition amount of the industrial grade-1 sponge titanium is as follows: 100-300 Kg of titanium sponge is added into a reaction vessel with the volume of per cubic meter.
4. The method for producing titanium sponge with low iron content and high quality as claimed in claim 1, wherein: in the step B, the operation of the titanizing treatment of the inner surface of the liquid magnesium vacuum ladle is as follows: placing the two-man ladle in a titanizing container, processing grade-1 sponge titanium in the titanizing container, connecting the titanizing container with a vacuum system, vacuumizing the titanizing container, starting an electric furnace when the vacuum degree of the titanizing container reaches 0.1-1 Pa, controlling the temperature to be 1000-1020 ℃, continuing for 30-60 hours, closing a temperature control system of the electric furnace, stopping the vacuum system when the temperature is reduced to 300 ℃, cooling to room temperature, and taking out the two-man ladle for later use.
5. The method for producing titanium sponge with low iron content and high quality as claimed in claim 4, wherein: when the liquid magnesium vacuum ladle is used for titanizing treatment, the addition amount of the industrial grade-1 sponge titanium is as follows: adding 100-300 Kg of titanium sponge into a titanizing container with the volume of per cubic meter.
6. The method for producing titanium sponge with low iron content and high quality as claimed in claim 1, wherein: in the step C, the adding amount of the liquid magnesium accounts for 70-80% of the volume of the reactor.
7. The method for producing titanium sponge with low iron content and high quality as claimed in any one of claims 1 to 6, wherein: in step C, the TiCl4The total addition amount of the magnesium is 2.0-2.3 times of the addition mass of the liquid magnesium.
8. The method for producing titanium sponge with high quality and low iron content as claimed in claim 7, wherein: in step C, the TiCl4Middle FeCl3The mass percentage content is 0.0003-0.0006%.
9. The method for producing titanium sponge with low iron content and high quality as claimed in any one of claims 1 to 6 or 8, wherein: the temperature of the vacuum distillation is 980-1020 ℃, the vacuum degree is 0.1-10 Pa, and the time is 70-90 hours.
10. The method for producing titanium sponge with high quality and low iron content as claimed in claim 7, wherein: the temperature of the vacuum distillation is 980-1020 ℃, the vacuum degree is 0.1-10 Pa, and the time is 70-90 hours.
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