CN112978792B - Method for separating magnetic artificial rutile from modified titanium slag - Google Patents

Method for separating magnetic artificial rutile from modified titanium slag Download PDF

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CN112978792B
CN112978792B CN202110243006.1A CN202110243006A CN112978792B CN 112978792 B CN112978792 B CN 112978792B CN 202110243006 A CN202110243006 A CN 202110243006A CN 112978792 B CN112978792 B CN 112978792B
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leaching
rutile
chromium
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张力
张晶
张伟
邹鑫
韩吉庆
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Northeastern University China
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • B03C1/02—Magnetic separation acting directly on the substance being separated
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    • C22B21/00—Obtaining aluminium
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    • C22B21/0023—Obtaining aluminium by wet processes from waste materials
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
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Abstract

The invention belongs to the field of artificial rutile production, and particularly relates to a method for separating magnetic artificial rutile from modified titanium slag. Comprises the steps of 1, selectively leaching at low temperature and chemically dissociating rutile phase; step 2, water leaching and strong magnetic separation of the artificial rutile concentrate; step 3, leaching and separating vanadium and chromium impurity components; and 3, carrying out water leaching separation on calcium and magnesium. NaHCO is used in the present application3With Na2CO3And low-temperature leaching is carried out, impurities in the boron-containing leaching solution are few, the boron component is easy to recover, and the calcium, magnesium, aluminum and silicon components are left in the leaching slag to create conditions for removing vanadium and chromium from the subsequent NaOH solution and recovering the aluminum component. According to the method, the rutile phase is leached by using a NaOH solution, the rutile phase is insoluble in alkali liquor, and impurities such as solid-dissolved vanadium, chromium and the like are dissolved in the alkali liquor, so that the content of the solid-dissolved vanadium and chromium impurities in the rutile phase is reduced, the residual components such as silicon, aluminum and the like in concentrate are further removed, the rutile quality is improved, and the low-vanadium-chromium artificial rutile is prepared. The low-calcium-magnesium artificial rutile is prepared by removing components such as calcium, magnesium and the like by water leaching.

Description

Method for separating magnetic artificial rutile from modified titanium slag
Technical Field
The invention belongs to the field of artificial rutile production, and particularly relates to a method for separating magnetic artificial rutile from modified titanium slag.
Background
Rutile is a high-quality raw material for producing titanium white, titanium sponge and welding rods, more than 90% of China depends on import, the external dependence is large, and the main source is Australia and Sera Freon. The content of CaO and MgO, vanadium and chromium and TiO in the titanium resources in China are high2Low grade, difficult direct preparationHigh-quality rutile is prepared. In order to provide guarantee for strategic safety of titanium resources in China, a new technology for preparing rutile by taking the titanium resources in China as raw materials is imperative to research and develop.
Chinese patent (CN201110072575.0) proposes a method for modifying titanium slag by melt oxidation and separating a rutile phase, and an artificial rutile with low CaO + MgO content is obtained by using flotation, reselection, high-concentration high-temperature alkaline leaching (NaOH leaching) and acid leaching processes as separation means, so as to realize separation of a rutile phase in modified titaniferous slag, but the method has the following disadvantages:
(1) flotation, gravity separation, high-alkali leaching (NaOH leaching and high-temperature leaching) and high-acid leaching are adopted as separation means, so that the problems of long flow, high cost, large occupied area, large investment, low separation index, difficult tailing utilization, small treatment capacity, large alkali consumption, serious equipment corrosion, high cost, large pollution and the like are solved;
(2) the rutile phase and the impurity phase are difficult to dissociate, and the gravity separation effect is poor;
(3) in the high-alkali high-temperature leaching process, silicate, silicon dioxide and the like enter the leaching solution, so that the alkali consumption is high and the cost is high;
(4) the high alkali leaching generates argillized silicate which is wrapped on the surface of the rutile phase, and the dissociation and mineral separation of the rutile phase are difficult;
(5) the ore grinding granularity is fine, the rutile granularity is small, the subsequent chlorination, the titanium white and the sponge titanium production are not facilitated, and the titanium yield is low;
(6) the modified slag has high silicon-aluminum component content, a large amount of colloid is generated by acid leaching, the subsequent filtration is extremely difficult, the subsequent filtration is difficult to carry out, and the cost is high;
(7) as artificial ore, the rutile phase is tightly combined with the matrix phase, the dissociation is difficult, and the subsequent gravity separation is not facilitated;
(8) the gravity separation process has large occupied area, poor separation efficiency and low yield;
(9) the flotation separation process has poor separation efficiency and large pollution, and tailings are difficult to utilize;
(10) impurities such as vanadium, chromium and the like are dissolved in the synthetic rutile phase in a solid solution manner and are difficult to remove, so that the quality of subsequent titanium and titanium sponge is influenced;
(11) the operation is complex and the industrialization is difficult.
Similarly, impurities such as vanadium, chromium and the like are also dissolved in the natural rutile phase in a solid manner and are difficult to remove, so that the quality of subsequent titanium and titanium sponge is influenced, and difficulty is brought to a subsequent impurity separation process.
Disclosure of Invention
In view of the problems, the method for separating the magnetic artificial rutile from the modified titanium slag is provided. The method takes modified titanium slag as a raw material and adopts NaHCO3With Na2CO3The solution is selectively leached at low temperature to obtain leached slag and boron-containing leachate, and the rutile phase in the leached slag is chemically dissociated. And separating leached residues by one or two of water leaching and strong magnetic separation to obtain artificial rutile concentrate and tailings. The artificial rutile or natural rutile concentrate is leached by NaOH, solid-dissolved impurities such as vanadium, chromium and the like are dissolved in alkali liquor to obtain low-vanadium-chromium artificial rutile concentrate, and then the low-calcium-magnesium artificial rutile concentrate is obtained by water leaching separation.
The boron-containing leachate and the vanadium-chromium-containing leachate are subjected to a recovery process to realize recovery of boron, vanadium, chromium, silicon and aluminum and realize circulation of alkali liquor.
The specific technical scheme is as follows: a method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and chemical dissociation of rutile phase:
modified titanium slag is taken as a raw material, NaHCO is adopted3、Na2CO3One or two of the solutions are combined to be used as leachate, selective leaching is carried out at low temperature, leaching residues and boron-containing leachate are obtained, and the rutile phase in the leaching residues is chemically dissociated; the leaching temperature is 20-50 ℃, boron leaching is promoted, and calcium, magnesium, silicon and aluminum are inhibited from entering boron-containing leachate;
the modified titanium slag is obtained by melting oxidation and component modification and tempering of titaniferous slag, and the component modification and tempering is to add B2O3Or adding B2O3With SiO2The titanium enters a rutile phase to form a titanium-rich phase, and other components enter an impurity phase which is one or two of a glass phase and a crystal phase;
step 2, water leaching and strong magnetic separation of leaching residues:
leaching slag is separated by one of water leaching or water leaching and strong magnetic separation combined processes to obtain artificial rutile concentrate, tailings or a water leaching solution:
the water leaching promotes calcium and magnesium to enter the leaching solution, and inhibits silicon-aluminum components from entering the leaching solution;
step 3, leaching and separating vanadium and chromium impurity components:
leaching the artificial rutile concentrate obtained in the step 2 by using a NaOH solution, allowing vanadium and chromium components dissolved in the artificial rutile phase to enter a vanadium-chromium leaching solution to obtain low-vanadium-chromium artificial rutile concentrate, and allowing silicon and aluminum in the artificial rutile concentrate to enter the vanadium-chromium leaching solution in the leaching process;
step 4, water leaching separation of the low-vanadium-chromium artificial rutile concentrate:
and (3) carrying out water leaching separation on the low-vanadium-chromium artificial rutile concentrate to promote calcium and magnesium to enter a leaching solution, so as to obtain the low-calcium-magnesium artificial rutile concentrate.
Further, B is added in the step 12O3With SiO2When, B2O3Is more than 40 wt% of the total mass of the mixture; when the content of metallic iron in the modified titanium slag is more than or equal to 1 wt%, separating iron by adopting weak magnetism, and then taking magnetic separation tailings as a leaching raw material; the particle size of the raw material is more than or equal to 78 mu m.
Further, the leaching conditions in the step 1 are that the liquid-solid ratio of the leaching solution to the raw material is 2-6 mL/g, and NaHCO is used3The mass ratio of the raw materials to the raw materials is 0.5-0.9, the stirring speed is 250-500 rpm, the leaching time is 30-80 min, the rutile phase dissociation degree in the leaching residues is more than or equal to 85%, the calcium leaching rate is less than or equal to 8%, the magnesium leaching rate is less than or equal to 5%, the silicon leaching rate is less than or equal to 3%, and the aluminum leaching rate is less than or equal to 5%.
Further, the step 1 also comprises the circulation of alkali leaching solution and the recovery of boron components:
and returning the boron-containing leachate to the leachate for circular leaching, when the total B concentration in the leachate is more than or equal to 6g/l, cooling the boron-containing leachate to room temperature, precipitating borax, returning the precipitated solution to the leachate for use, or directly using the solution as the leachate after heating and concentrating, wherein the boron recovery rate is more than or equal to 90%.
Further, the strong magnetic separation in the step 2 is to separate a weak magnetic rutile phase; when the content of metallic iron in the artificial rutile concentrate is more than or equal to 1 percent, weak magnetism is adopted to separate iron.
Further, TiO in the synthetic rutile concentrate in the step 22The content of the calcium-magnesium-calcium-magnesium alloy is 91-98 wt%, the content of CaO and MgO is 0.8-1.2 wt%, the recovery rate of titanium is more than or equal to 80%, the leaching rate of calcium is more than or equal to 80%, the leaching rate of magnesium is more than or equal to 60%, the leaching rate of silicon is less than or equal to 2%, and the leaching rate of aluminum is less than or equal to 5%.
Further, in the step 3, the leaching conditions of the NaOH solution are that the solid-to-solid ratio of the NaOH solution to the synthetic rutile concentrate is 2-10 mL/g, the leaching temperature is 50-100 ℃, the mass concentration of the NaOH leachate is 30-50%, the stirring speed is 250-600 rpm, and the leaching time is 30-60 min.
Further, the low vanadium chromium synthetic rutile obtained in step 3 has a total V content of <0.5 wt%, a total Cr content of <0.5 wt%, a total aluminum content of <0.5 wt%, and a total silicon content of <1.2 wt%.
The water leaching conditions of the step 2 and the step 4 are that the liquid-solid ratio is 3-11 mL/g, the water leaching temperature is 90-100 ℃, the stirring speed is 600-800 rpm, and the leaching time is 60-120 min; and 4, leaching and removing the calcium and magnesium components by hydrochloric acid when the CaO + MgO content in the low-calcium magnesium artificial rutile is less than or equal to 0.6 wt% and the CaO + MgO content is more than 0.6 wt%.
Leaching natural rutile concentrate with NaOH solution, and allowing vanadium and chromium dissolved in natural rutile phase to enter vanadium-chromium leaching solution to obtain low-vanadium-chromium rutile; the total V content in the low-vanadium chromium artificial rutile is less than 0.5 wt%, and the total Cr content is less than 0.5 wt%; the leaching conditions of the NaOH solution are that the solid-to-solid ratio of the NaOH solution to the natural rutile concentrate is 2-10 mL/g, the leaching temperature is 50-100 ℃, the mass concentration of the NaOH leachate is 30-50%, the stirring speed is 250-800 rpm, and the leaching time is 30-60 min.
The principle and the beneficial effects of the invention are as follows:
(1) principle and beneficial effect of low-temperature selective leaching
Firstly, only the boron component is leached, other components are not leached, including silicate phase, silicon dioxide, aluminum oxide and the like, the alkali consumption is low, the cost is low, the impurities in the leaching solution are few, the boron component is easy to recover, and the operation is simple;
secondly, the cost is far lower than that of NaOH, the cost is low, and the environment is friendly;
the corrosion of the equipment is small, the cost is low, and the investment is small;
the phase interface of the rutile phase and the matrix phase is broken, the dissociation degree of the rutile phase is improved, and conditions are created for subsequent breaking dissociation and strong magnetic separation;
fifthly, calcium and magnesium in the slag are dissociated and become free, low-temperature leaching inhibits free calcium and magnesium components from entering the leaching solution, impurities in the boron-containing leaching solution are reduced, recycling is easy, and aluminum components are left in the leaching slag to create conditions for removing vanadium and chromium through NaOH solution and recycling the aluminum components.
(2) Principle and beneficial effect of leaching residue water leaching or strong magnetic separation
Firstly, based on the water leaching principle, after low-temperature leaching in the step 1, calcium and magnesium in the slag are dissociated to form a free state which is distributed on the surface of the rutile phase, so that the dissociation degree and the magnetic separation of the rutile phase are influenced. By adopting water leaching separation, the pH is reduced, calcium and magnesium distributed on the surface of the rutile phase are dissolved into the leaching solution, the dissociation and magnetism of the rutile phase are increased, and the magnetic separation effect is improved.
The water leaching separation reduces the content of CaO and MgO in the rutile concentrate, and creates conditions for the subsequent production of titanium white and titanium sponge. The water leaching is low in cost, clean, efficient and environment-friendly.
Secondly, on the strong magnetic principle, impurities such as vanadium, chromium, iron, manganese, cobalt, nickel and the like are dissolved or mixed in the rutile phase, and the rutile phase has weak magnetism;
the strong magnetic separation process is adopted, so that the method is clean, efficient, low in cost, high in ore efficiency, low in cost and environment-friendly, the amount of minerals entering the alkaline leaching process is greatly reduced, and the alkaline consumption and the cost are reduced;
(3) principle and beneficial effect of removing vanadium and chromium by NaOH solution
Firstly, impurities such as vanadium, chromium and the like dissolved in rutile phase are difficult to remove, and the quality of subsequent titanium and titanium sponge is influenced;
leaching with NaOH solution, wherein the rutile phase is insoluble in alkali liquor, and impurities such as solid-dissolved vanadium, chromium and the like are soluble in alkali liquor, so that the content of the solid-dissolved vanadium-chromium impurities in the rutile phase is reduced, residual components such as silicon, aluminum and the like in concentrate are further removed, the rutile quality is improved, the low-vanadium-chromium artificial rutile is prepared, conditions are created for subsequent chlorination, refining, titanium white and titanium sponge production, and the titanium white and titanium sponge quality is improved;
thirdly, the content of impurities such as silicon, aluminum and the like in the artificial rutile concentrate obtained in the step 2 is low, NaOH solution is adopted for leaching, the alkali consumption is low, the cost is low, and after cyclic leaching, the vanadium-chromium leaching solution is used as a raw material for extracting vanadium-chromium-aluminum-silicon, so that the comprehensive recovery of vanadium-chromium-aluminum-silicon components can be realized;
calcium and magnesium in the slag are further dissociated to form free state which is distributed on the surface of rutile phase, thereby creating conditions for the subsequent water leaching process.
(4) Water leaching principle and beneficial effect of low-vanadium-chromium artificial rutile
The water leaching separation is adopted, the pH is reduced, calcium and magnesium distributed on the surface of rutile phase are dissolved and enter a leaching solution, the content of CaO and MgO is reduced, and conditions are created for the subsequent production of titanium white and titanium sponge.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is an SEM image of the raw material-modified slag of example 1.
FIG. 3 is an XRD pattern (1, rutile) of the raw material-modified slag of example 1.
Figure 4 is the XRD pattern of the low vanadium chromium and low calcium magnesium synthetic rutile concentrate of the product of example 1.
Detailed Description
The present invention will be further described with reference to specific examples, which are, of course, only a few examples and are not intended to represent all embodiments of the present invention.
Example 1
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and chemical dissociation of rutile phase:
the modified titanium slag is used as a raw material, the components are shown in Table 1, and TiO2Grade 63.34 wt%, using Na2CO3With NaHCO3Selectively leaching at low temperature to obtain leaching residue and boron-containing leaching solution, wherein the dissociation degree of rutile phase in the leaching residue is 97%, the leaching rate of calcium is 5.6%, the leaching rate of magnesium is 4.6%, the leaching rate of silicon is 1.7%, and the leaching rate of aluminum is 4.1%; the leaching conditions are that the liquid-solid ratio is 2, the leaching temperature is 20 ℃, the pH value of the leaching solution is 8.0, the ratio of alkali to raw materials is 0.5, the stirring speed is 250rpm, and the leaching time is 30 min.
TABLE 1 chemical composition of modified slag (wt%)
Figure BDA0002962986050000061
Returning the boron-containing leachate to the step 1 for circular leaching, cooling the boron-containing leachate to room temperature after 18g/l is reached, precipitating borax, returning the precipitated solution to the step 1 for use, and ensuring that the recovery rate of boron components is 99%;
the modified titanium slag is obtained by melting and oxidizing titaniferous slag and quenching and tempering components, wherein the quenching and tempering components are obtained by adding B2O3The titanium component enters a rutile phase to form a titanium-rich phase, and the impurity phase is a glass phase;
step 2, leaching and separating leaching residues:
leaching slag is subjected to a water leaching and strong magnetism combined separation process to obtain artificial rutile concentrate and tailings, and TiO in the artificial rutile concentrate297 wt% of the total amount of CaO and MgO, 0.80 wt% of the total amount of vanadium, 0.3 wt% of the total amount of chromium, a titanium recovery rate of not less than 99%, a calcium leaching rate of 95%, a magnesium leaching rate of 85%, a silicon leaching rate of 1.2%, and an aluminum leaching rate of 1.9%; the water leaching conditions are that the liquid-solid ratio is 11, the leaching temperature is 100 ℃, the stirring speed is 800rpm, and the leaching time is 120 min.
Step 3, leaching and separating vanadium and chromium impurity components:
leaching the synthetic rutile concentrate with NaOH solution to obtain low-vanadium-chromium synthetic rutile; the leaching conditions of the NaOH solution are that the liquid-solid ratio is 6, the leaching temperature is 50 ℃, the concentration (mass concentration) of the leaching solution is 50%, the stirring speed is 250rpm, and the leaching time is 30 min;
the low-vanadium chromium artificial rutile contains less than 0.1 wt% of total V and less than 0.1 wt% of total Cr.
Step 4, calcium and magnesium water leaching separation:
the low-vanadium-chromium artificial rutile is subjected to a water leaching process to obtain low-calcium-magnesium artificial rutile concentrate, the chemical components of which are shown in table 2, and the content of CaO and MgO in the concentrate is less than or equal to 0.6 wt%; the water leaching conditions are that the liquid-solid ratio is 5, the leaching temperature is 100 ℃, the leaching time is 120nin, and the stirring speed is 800 rpm.
TABLE 2 chemical composition of low calcium magnesium and low vanadium chromium synthetic rutile concentrate (wt%)
Figure BDA0002962986050000071
Example 2
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and rutile phase chemical dissociation:
takes modified titanium slag as raw material and TiO2The grade is 72 wt%, NaHCO is adopted3Selectively leaching at low temperature to obtain leaching residue and boron-containing leaching solution, wherein the dissociation degree of rutile phase in the leaching residue is 85%, the recovery rate of boron components is 90%, the leaching rate of calcium is 54.5%, the leaching rate of magnesium is 3.7%, the leaching rate of silicon is 1.7%, and the leaching rate of aluminum is 4.0%; the leaching conditions are that the liquid-solid ratio is 6, the leaching temperature is 50 ℃, the pH value of the leaching solution is 7.8, the ratio of alkali to raw materials is 0.5, the stirring speed is 500rpm, and the leaching time is 80 min.
Returning the boron-containing leachate to the step 1 for circular leaching, cooling the boron-containing leachate to room temperature after 12g/l is reached, precipitating borax, and directly using the precipitated solution as the leachate in the step 1 after heating and concentrating;
the modified titanium slag is obtained by melting and oxidizing titaniferous slag and quenching and tempering components, wherein the quenching and tempering components are obtained by adding B2O3With SiO2，B2O3The addition amount is 40 wt%, and the titanium component enters into rutile phase to form titanium-rich phaseThe impurity phase is a glass phase;
step 2, leaching and strong magnetic separation of leaching residues:
leaching slag is subjected to a water leaching separation combined process to obtain artificial rutile concentrate and tailings, and TiO in the artificial rutile concentrate296 percent of the leaching agent, 1.2 percent of CaO and MgO, 1.0 percent of vanadium, 0.5 percent of chromium, more than or equal to 90 percent of titanium recovery rate, 89 percent of calcium leaching rate, 71 percent of magnesium leaching rate, 1.8 percent of silicon leaching rate and 3.9 percent of aluminum leaching rate; the water leaching conditions are that the liquid-solid ratio is 11, the leaching temperature is 100 ℃, the stirring speed is 800rpm, and the leaching time is 40 min.
Step 3, leaching and separating vanadium and chromium impurity components
Leaching the synthetic rutile concentrate with NaOH solution to obtain low-vanadium-chromium synthetic rutile; the leaching conditions of the NaOH solution are that the liquid-solid ratio is 10, the leaching temperature is 100 ℃, the concentration (mass concentration) of the leaching solution is 50 percent, and the stirring speed is 600 rpm; the low-vanadium chromium artificial rutile contains 0.2 wt% of total V and 0.1 wt% of total Cr.
After the vanadium-chromium leaching solution is circularly leached, the leaching solution is used as a raw material for extracting vanadium and chromium;
step 4, calcium and magnesium water leaching separation:
the low-vanadium-chromium artificial rutile is subjected to a water leaching process to obtain low-calcium-magnesium artificial rutile concentrate, wherein the content of CaO and MgO in the concentrate is less than or equal to 0.6 wt%; the water leaching conditions are that the liquid-solid ratio is 3, the leaching temperature is 100 ℃, the stirring speed is 600rpm, and the leaching time is 120 min.
Example 3
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and rutile phase chemical dissociation:
modified titanium slag TiO2Grade of 10 wt%, using Na2CO3Selectively leaching at low temperature to obtain leaching residue and boron-containing leaching solution, wherein the dissociation degree of rutile phase in the leaching residue is 85%, the recovery rate of boron components is 90%, the leaching rate of calcium is 7.8%, the leaching rate of magnesium is 4.9%, the leaching rate of silicon is 3.0%, and the leaching rate of aluminum is 4.8%; the leaching condition is thatThe solid ratio is 3, the leaching temperature is 30 ℃, the pH value of the leaching solution is 9.0, the ratio of alkali to raw materials is 0.5, the stirring speed is 300rpm, and the leaching time is 30 min.
Returning the boron-containing leachate to the step 1 for circular leaching, cooling the boron-containing leachate to room temperature after 15g/l is reached, precipitating borax, and returning the precipitated solution to the step 1 for use;
the modified titanium slag is obtained by melting and oxidizing titaniferous slag and quenching and tempering components, wherein the quenching and tempering components are obtained by adding B2O3The titanium component enters a rutile phase to form a titanium-rich phase, and the impurity phase is a glass phase;
step 2, leaching and strong magnetic separation of leaching residues:
leaching residues are subjected to a water leaching-strong magnetic separation combined process to obtain artificial rutile concentrate and tailings, wherein the artificial rutile concentrate contains 91 wt% of CaO and MgO, 0.6 wt% of vanadium, 0.8 wt% of chromium, 80% of titanium, 80% of calcium, 61% of magnesium, 1.9% of silicon and 4.0% of aluminum; the water leaching conditions are that the liquid-solid ratio is 6, the leaching temperature is 100 ℃, the stirring speed is 800rpm, and the leaching time is 100 min.
Step 3, leaching and separating the vanadium and chromium components:
leaching the synthetic rutile concentrate with NaOH solution to obtain low-vanadium-chromium synthetic rutile; the leaching conditions of the NaOH solution are that the liquid-solid ratio is 2, the leaching temperature is 100 ℃, the concentration (mass concentration) of the leaching solution is 40%, the stirring speed is 600rpm, and the leaching time is 50 min;
the low-vanadium chromium artificial rutile contains 0.1 wt% of total V and 0.2 wt% of total Cr.
After the vanadium-chromium leaching solution is circularly leached, the leaching solution is used as a raw material for extracting vanadium and chromium;
step 4, calcium and magnesium water leaching separation:
the low-vanadium-chromium artificial rutile is subjected to a water leaching process to obtain low-calcium-magnesium artificial rutile concentrate, wherein the content of CaO and MgO in the concentrate is less than or equal to 0.6 wt%; the water leaching conditions are that the liquid-solid ratio is 11, the leaching temperature is 90 ℃, the stirring speed is 800rpm, and the leaching time is 100 min.
Example 4
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and rutile phase chemical dissociation:
takes modified titanium slag as raw material and TiO2Grade of 80 wt%, using Na2HCO3Selectively leaching at low temperature to obtain leaching residue and boron-containing leaching solution, wherein the dissociation degree of rutile phase in the leaching residue is 96%, the recovery rate of boron components is 97%, the leaching rate of calcium is 3.8%, the leaching rate of magnesium is 3.1%, the leaching rate of silicon is 1.8%, and the leaching rate of aluminum is 3.4%; the leaching conditions are that the liquid-solid ratio is 6, the leaching temperature is 40 ℃, the pH value of the leaching solution is 7.6, the ratio of alkali to raw materials is 0.9, the stirring speed is 400rpm, and the leaching time is 60 min.
Returning the boron-containing leachate to the step 1 for circular leaching, cooling the boron-containing leachate to room temperature after 20g/l is reached, precipitating borax, and returning the precipitated solution to the step 1 for use;
the modified titanium slag is obtained by melting and oxidizing titaniferous slag and quenching and tempering components, wherein the quenching and tempering components are obtained by adding B2O3The titanium component enters a rutile phase to form a titanium-rich phase, and the impurity phase is a glass phase;
step 2, leaching and strong magnetic separation of leaching residues:
leaching slag is subjected to a water leaching-strong magnetic separation combined process to obtain artificial rutile concentrate and tailings, and TiO in the artificial rutile concentrate297 wt% of the total amount of CaO and MgO, 1.2 wt% of the total amount of vanadium, 0.1 wt% of the total amount of chromium, 80% of the recovery rate of titanium, 80% of the leaching rate of calcium, 60% of the leaching rate of magnesium, 1.7% of the leaching rate of silicon and 3.6% of the leaching rate of aluminum; the water leaching conditions are that the liquid-solid ratio is 9, the water leaching temperature is 100 ℃, the stirring speed is 800rpm, and the leaching time is 80 min.
Step 3, leaching and separating the vanadium and chromium components:
leaching the synthetic rutile concentrate with NaOH solution to obtain low-vanadium-chromium synthetic rutile; the leaching conditions of the NaOH solution are that the liquid-solid ratio is 3, the leaching temperature is 100 ℃, the concentration (mass concentration) of the leaching solution is 50%, the stirring speed is 300rpm, and the leaching time is 30 min; the low-vanadium chromium artificial rutile contains less than 0.1 wt% of total V and less than 0.1 wt% of total Cr.
Returning the vanadium-chromium leaching solution to the step 4, and performing circulating leaching to obtain a leaching solution serving as a raw material for vanadium-chromium extraction;
step 4, calcium and magnesium water leaching separation:
the low-vanadium-chromium artificial rutile is subjected to a water leaching process to obtain low-calcium-magnesium artificial rutile concentrate, wherein the content of CaO and MgO in the concentrate is 0.6 wt%; the water leaching conditions are that the liquid-solid ratio is 3, the leaching temperature is 100 ℃, the stirring speed is 700rpm, and the leaching time is 110 min.
Example 5
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
step 1, low-temperature selective leaching and rutile phase chemical dissociation:
takes modified titanium slag as raw material and TiO2Grade 75 wt%, using Na2CO3With Na2HCO3Selectively leaching to obtain leaching residue and boron-containing leaching solution, wherein the dissociation degree of rutile phase in the leaching residue is 94%, the recovery rate of boron components is 96%, the leaching rate of calcium is 4.8%, the leaching rate of magnesium is 3.7%, the leaching rate of silicon is 2.4%, and the leaching rate of aluminum is 4.0%; the leaching conditions are that the liquid-solid ratio is 5, the leaching temperature is 30 ℃, the pH value of the leaching solution is 8.5, the ratio of alkali to raw materials is 0.9, the stirring speed is 400rpm, and the leaching time is 50 min;
returning the boron-containing leachate to the step 1 for circular leaching, cooling the boron-containing leachate to room temperature after 15g/l is reached, precipitating borax, and returning the precipitated solution to the step 1 for use;
the modified titanium slag is obtained by melting and oxidizing titaniferous slag and quenching and tempering components, wherein the quenching and tempering components are obtained by adding B2O3The titanium component enters a rutile phase to form a titanium-rich phase, and the impurity phase is a glass phase;
step 2, leaching and strong magnetic separation of leaching residues:
leaching slag is subjected to a water leaching-strong magnetic separation combined process to obtain artificial rutile concentrate and tailings and artificial rutile concentrate TiO296 wt%, CaO + MgO 0.8 wt%, vanadium 0.5 wt%, and chromium 0.3 w%t%, the recovery rate of titanium is 81%, the leaching rate of calcium is 83%, the leaching rate of magnesium is 61%, the leaching rate of silicon is 1.3%, and the leaching rate of aluminum is 3.2%; the water leaching conditions are that the liquid-solid ratio is 3, the water leaching temperature is 90 ℃, the stirring speed is 700rpm, and the leaching time is 90 min.
Step 3, leaching and separating vanadium and chromium impurity components
Leaching the synthetic rutile concentrate with NaOH solution to obtain low-vanadium-chromium synthetic rutile; the leaching conditions of the NaOH solution are that the liquid-solid ratio is 3, the leaching temperature is 90 ℃, the concentration (mass concentration) of the leaching solution is 40%, the stirring speed is 500rpm, and the leaching time is 40 min; after the vanadium-chromium leaching solution is circularly leached, the leaching solution is used as a raw material for extracting vanadium and chromium.
The low-vanadium chromium artificial rutile contains less than 0.1 wt% of total V and less than 0.1 wt% of total Cr.
Step 4, calcium and magnesium water leaching separation:
the low-vanadium-chromium artificial rutile is subjected to a water leaching process to obtain low-calcium-magnesium artificial rutile concentrate, wherein the content of CaO and MgO in the concentrate is 0.7 wt%; the water leaching conditions are that the liquid-solid ratio is 8, the leaching temperature is 100 ℃, the stirring speed is 800rpm, and the leaching time is 110 min; the concentrate with the CaO and MgO content of 0.7 wt% is leached by hydrochloric acid, the CaO and MgO content is 0.2 wt%, the hydrochloric acid leaching condition is that the liquid-solid ratio is 3, the water leaching temperature is 20 ℃, the stirring speed is 250rpm, the hydrochloric acid concentration is 1 wt%, and the leaching time is 10 min.
Example 6
A method for separating magnetic artificial rutile from modified titanium slag comprises the following steps:
leaching separation of vanadium and chromium impurity components
The content of all V in the natural rutile concentrate is 0.8 wt%, the content of all Cr is 0.2 wt%, the natural rutile concentrate is leached by NaOH solution, vanadium and chromium which are solid-dissolved in the natural rutile phase enter vanadium-chromium leaching solution, and natural low-vanadium-chromium rutile is obtained; the leaching conditions of the NaOH solution are that the solid-to-solid ratio of the NaOH solution to the natural rutile concentrate is 6mL/g, the leaching temperature is 100 ℃, the mass concentration of the NaOH leaching solution is 40%, the stirring speed is 600rpm, and the leaching time is 60 min. After the vanadium-chromium leaching solution is circularly leached, the leaching solution is used as a raw material for extracting vanadium and chromium.
The low-vanadium chromium natural rutile contains less than 0.1 wt% of total V and less than 0.1 wt% of total Cr.
Comparative example 1
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in the example 1, except that:
in step 1, Na is used2CO3With NaHCO3Leaching at low temperature to obtain leaching slag and boron-containing leaching liquid. The leaching conditions are that the liquid-solid ratio is 2, the leaching temperature is 120 ℃, the pH value of the leaching solution is 8.0, the ratio of alkali to raw materials is 0.5, the stirring speed is 250rpm, and the leaching time is 30 min.
The leaching result is that the leaching rate of calcium is more than or equal to 80 percent, the leaching rate of magnesium is more than or equal to 47 percent, the leaching rate of silicon is more than or equal to 5 percent, the leaching rate of aluminum is more than or equal to 62 percent, a large amount of calcium, magnesium, silicon, aluminum and silicon enter the boron-containing leaching solution, on one hand, the subsequent recovery of boron is difficult, on the other hand, a large amount of alkali is consumed by silicon-aluminum components, the cost is increased, the aluminum components cannot be recycled, and meanwhile, the leaching temperature is increased, and equipment is corroded.
Comparative example 2
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in the example 2, except that:
in the step 2, the leached slag does not have a water leaching process, and is directly subjected to strong magnetic separation, so that the content of CaO and MgO in the obtained artificial rutile is 4.5 wt%.
The direct strong magnetism can not remove calcium and magnesium, which brings difficulty to the removal of calcium and magnesium components in the subsequent step 4, so that the product can not be used as a raw material for boiling chlorination (the boiling chlorination process requirement is less than or equal to 1.2 wt%), because the content of CaO and MgO seriously exceeds the standard, MgCl is generated in the chlorination process2With CaCl2The raw materials are sintered and boiling chlorination cannot be carried out.
Comparative example 3
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in the example 2, except that:
in the step 2, the leaching condition of the leaching residue is that the liquid-solid ratio is 2, the leaching temperature is 30 ℃, the stirring speed is 250rpm, and the content of CaO and MgO in the obtained artificial rutile concentrate is 4.5wt percent
The content of CaO and MgO exceeds the standard, so that the product cannot be used as a raw material for boiling chlorination (the requirement of the boiling chlorination process is less than or equal to 1.2wt percent), because MgCl is generated in the chlorination process2With CaCl2The raw materials are sintered and boiling chlorination cannot be carried out.
Comparative example 4
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in the example 6, except that:
in the vanadium-chromium leaching separation process in the step 3, the leaching conditions of the NaOH solution are as follows: the liquid-solid ratio is 3, the leaching temperature is 100 ℃, the concentration (mass concentration) of the leaching solution is 15 percent, and the stirring speed is 300 rpm.
The artificial rutile concentrate obtained by the method has the vanadium content of 0.6 wt%, the chromium content of 0.8 wt%, the titanium recovery rate of 80%, the calcium leaching rate of 80%, the magnesium leaching rate of 61%, the silicon leaching rate of 1.9% and the aluminum leaching rate of 4.0%.
The method can not remove vanadium and chromium dissolved in the artificial rutile phase, and the obtained artificial rutile concentrate has high vanadium and chromium content, thereby bringing difficulties to the subsequent titanium dioxide production and sponge titanium production and TiCl4The vanadium-chromium impurity removal process in the refining process brings great difficulty, so that titanium white products turn yellow, and titanium sponge becomes brittle, and the titanium sponge becomes unqualified products.
Comparative example 5
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in example 4, except that:
the calcium and magnesium water leaching separation step in the step 4 is not carried out, the calcium and magnesium cannot be removed, the content of CaO and MgO in the obtained artificial rutile concentrate is 1.5 wt%, so that the product cannot be used as a raw material for boiling chlorination (the boiling chlorination process requirement is less than or equal to 1.2 wt%), and MgCl is generated in the chlorination process because the content of CaO and MgO exceeds the standard2With CaCl2The raw materials are sintered and boiling chlorination cannot be carried out.
Comparative example 6
The method for separating the magnetic artificial rutile from the modified titanium slag is the same as the method in the example 6, except that:
the total V content in the natural rutile concentrate was 0.8 wt%, the total Cr content was 0.2 wt%, and the NaOH solution leaching separation process of step 3 was not performed.
The total V content in the finally obtained natural rutile concentrate is 0.8 wt%, the total Cr content is 0.2 wt%, the subsequent titanium white production and the titanium sponge production are difficult, and TiCl is difficult4The vanadium-chromium impurity removal process in the refining process brings great difficulty, so that titanium white products turn yellow, and titanium sponge becomes brittle, and the titanium sponge becomes unqualified products.

Claims (6)

1. A method for separating magnetic artificial rutile from modified titanium slag is characterized by comprising the following steps:
step 1, low-temperature selective leaching and chemical dissociation of rutile phase:
modified titanium slag is taken as a raw material, NaHCO is adopted3、Na2CO3One or two of the solutions are combined to be used as leachate, selective leaching is carried out at low temperature, leaching residues and boron-containing leachate are obtained, and the rutile phase in the leaching residues is chemically dissociated; the leaching temperature is 20-50 ℃, boron leaching is promoted, and calcium, magnesium, silicon and aluminum are inhibited from entering boron-containing leachate;
the modified titanium slag is obtained by melting oxidation and component modification and tempering of titaniferous slag, and the component modification and tempering is to add B2O3Or adding B2O3With SiO2The titanium enters a rutile phase to form a titanium-rich phase, and other components enter an impurity phase which is one or two of a glass phase and a crystal phase;
step 2, water leaching and strong magnetic separation of leaching residues:
leaching slag is separated by one of water leaching or water leaching and strong magnetic separation combined processes to obtain artificial rutile concentrate, tailings or a water leaching solution:
the water leaching promotes calcium and magnesium to enter the leaching solution, and inhibits silicon-aluminum components from entering the leaching solution;
step 3, leaching and separating vanadium and chromium impurity components:
leaching the artificial rutile concentrate obtained in the step 2 by using a NaOH solution, allowing vanadium and chromium components dissolved in the artificial rutile phase to enter a vanadium-chromium leaching solution to obtain low-vanadium-chromium artificial rutile concentrate, and allowing silicon and aluminum in the artificial rutile concentrate to enter the vanadium-chromium leaching solution in the leaching process;
step 4, water leaching separation of the low-vanadium-chromium artificial rutile concentrate:
carrying out water leaching separation on the low-vanadium-chromium artificial rutile concentrate to promote calcium and magnesium to enter a leaching solution, so as to obtain the low-calcium-magnesium artificial rutile concentrate;
the leaching conditions of the step 1 are that the liquid-solid ratio of the leaching solution to the raw material is 2-6 mL/g, and NaHCO is used3The mass ratio of the raw materials to the raw materials is 0.5-0.9, the stirring speed is 250-500 rpm, the leaching time is 30-80 min, the rutile phase dissociation degree in the leaching residues is more than or equal to 85%, the calcium leaching rate is less than or equal to 8%, the magnesium leaching rate is less than or equal to 5%, the silicon leaching rate is less than or equal to 3%, and the aluminum leaching rate is less than or equal to 5%;
the water leaching conditions of the step 2 and the step 4 are that the liquid-solid ratio is 3-11 mL/g, the water leaching temperature is 90-100 ℃, the stirring speed is 600-800 rpm, and the leaching time is 60-120 min; the content of CaO and MgO in the low-calcium-magnesium artificial rutile obtained in the step (4) is less than or equal to 0.6 wt%, and when the content of CaO and MgO is more than 0.6 wt%, calcium and magnesium components are leached out and removed by hydrochloric acid;
in the step 3, the leaching conditions of the NaOH solution are that the solid-to-solid ratio of the NaOH solution to the artificial rutile concentrate is 2-10 mL/g, the leaching temperature is 50-100 ℃, the mass concentration of the NaOH leaching solution is 30-50%, the stirring speed is 250-600 rpm, and the leaching time is 30-60 min.
2. The method for separating magnetic synthetic rutile from modified titanium slag as claimed in claim 1, wherein B is added in step 12O3With SiO2When, B2O3Is more than 40 wt% of the total mass of the mixture; when the content of metallic iron in the modified titanium slag is more than or equal to 1 wt%, separating iron by adopting weak magnetism, and then taking magnetic separation tailings as a leaching raw material; the particle size of the raw material is more than or equal to 78 mu m.
3. The method for separating magnetic synthetic rutile from modified titanium slag according to claim 1, wherein the step 1 further comprises the steps of recycling alkaline leach liquor and recovering boron components:
and returning the boron-containing leachate to the leachate for circular leaching, when the total B concentration in the leachate is more than or equal to 6g/l, cooling the boron-containing leachate to room temperature, precipitating borax, returning the precipitated solution to the leachate for use, or directly using the solution as the leachate after heating and concentrating, wherein the boron recovery rate is more than or equal to 90%.
4. The method for separating the magnetic artificial rutile from the modified titanium slag as claimed in claim 1, wherein the strong magnetic separation in step 2 is separation of a weak magnetic rutile phase; when the content of metallic iron in the artificial rutile concentrate is more than or equal to 1 percent, weak magnetism is adopted to separate iron.
5. The method of claim 1, wherein the step 2 is performed by using TiO in the concentrate of artificial rutile2The content of the calcium-magnesium-calcium-magnesium alloy is 91-98 wt%, the content of CaO and MgO is 0.8-1.2 wt%, the recovery rate of titanium is more than or equal to 80%, the leaching rate of calcium is more than or equal to 80%, the leaching rate of magnesium is more than or equal to 60%, the leaching rate of silicon is less than or equal to 2%, and the leaching rate of aluminum is less than or equal to 5%.
6. The method for separating magnetic artificial rutile from the modified titanium slag as claimed in claim 1, wherein the low vanadium chromium artificial rutile obtained in step 3 has a total V content of <0.5 wt%, a total Cr content of <0.5 wt%, a total Al content of <0.5 wt% and a total Si content of <1.2 wt%.
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