CN112609075A - Titanium chloride dust collection slag treatment process - Google Patents

Titanium chloride dust collection slag treatment process Download PDF

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CN112609075A
CN112609075A CN202011351807.1A CN202011351807A CN112609075A CN 112609075 A CN112609075 A CN 112609075A CN 202011351807 A CN202011351807 A CN 202011351807A CN 112609075 A CN112609075 A CN 112609075A
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solution
treatment process
chloride
collecting slag
concentration
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何向阳
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Feichao Shanghai Environmental Technology Co ltd
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Abstract

The invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acid solution to form mixed slurry; and then filtering the mixed slurry to form a solid and a metal chloride solution, and washing and filtering the solid for multiple times to obtain a product I. And extracting the metal chloride solution by using an extracting agent to separate an iron chloride water phase, adding alkali liquor into the first oil phase, and performing back extraction, aging and centrifugal separation to obtain a product II. And (3) introducing chlorine gas into the iron chloride water phase to prepare an iron trichloride solution, and then adding aluminum hydroxide to prepare a third product. Different products are formed after the titanium chloride dust-collecting slag is treated, the cyclic utilization, the reduction and the harmless treatment of resources are realized, compared with the prior art, the acid-base neutralization treatment is adopted, the use of a large amount of base is saved, the fund is saved, and the treatment process effectively utilizes the chlorine generated in the production of the titanium dioxide and is more environment-friendly.

Description

Titanium chloride dust collection slag treatment process
Technical Field
The invention relates to the technical field of solid waste purification treatment, in particular to a titanium chloride dust-collecting slag treatment process.
Background
Titanium tetrachloride is an intermediate raw material for producing titanium dioxide and sponge titanium by a chlorination process, and is also a main raw material for preparing other titanium dioxide products. The raw material for producing the titanium tetrachloride is titanium-containing raw material such as high titanium slag, natural rutile or artificial rutile, and the raw material reacts with carbon and chlorine to generate the titanium tetrachloride and simultaneously generate solid dust slag containing metal chloride. The titanium chloride dust-collecting slag mainly comprises ferric chloride, aluminum trichloride, manganese dichloride, calcium chloride, magnesium chloride, titanium tetrachloride, zirconium tetrachloride, vanadyl dichloride, titanium dioxide, silicon dioxide, carbon and the like. The chlorinated dust-collecting slag with the composition is easy to hydrolyze and volatilize, can generate a large amount of harmful smoke when exposed to the air, and can form acid water and hydrochloric acid gas bodies when dissolved in water.
At present, most of titanium chloride dust-collecting slag treatment methods adopt treatment measures such as direct landfill and stockpiling, slurried deep underground injection, solid slag landfill after neutralization and the like. For example, the Chinese patent application with the publication number of CN100998914A discloses a method for treating low-grade titanium-rich chloride dust-collecting slag, which adopts lime neutralization reaction, and then carries out filtration and washing to finally obtain calcium chloride. Chinese patent application with publication number CN108892179A discloses a method for green treatment of titanium tetrachloride dust-collecting slag, which obtains Fe by filtering, concentrating and roasting2O3Powder and titanium slag.
The treatment measures are only the transfer of the chlorination residues or the conversion of the types of pollutants, and the complete purification treatment of other metal substances in the titanium chloride dust collecting residues is not carried out fundamentally, so that the pollution threat of the dust residues to the environment exists all the time.
In view of the above, there is a need to improve the treatment method of titanium chloride dust-collecting slag in the prior art to solve the above problems.
Disclosure of Invention
The invention aims to disclose a titanium chloride dust-collecting slag treatment process, which separates each component substance in the titanium chloride dust-collecting slag through the steps of filtering, extracting, back-extracting, centrifugal separation and the like, finally obtains three different products, realizes the effective utilization of resources, more thoroughly treats the titanium chloride dust-collecting slag, and ensures that the formed products can not influence the environment so as to solve the problem that the titanium chloride dust-collecting slag can not be effectively treated in the prior art.
In order to realize the aim, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acid solution to form mixed slurry;
step two: filtering the mixed slurry to form solids and a metal chloride solution, wherein the solids comprise titanium dioxide, silicon dioxide and carbon;
step three: washing and filtering the solid in the step two for multiple times to obtain a product I;
step four: extracting the metal chloride solution in the step two to separate an iron chloride water phase and a first oil phase;
step five: adding alkali liquor into the first oil phase in the fourth step, and preparing a first alkaline solution through back extraction;
step six: aging the first alkaline solution in the fifth step;
step seven: centrifuging the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product;
step eight: adding a strong acid into the second oil phase in the step seven, adjusting the pH value to form a new extracting agent, returning the new extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to form a new acidic solution, and returning the new acidic solution to the step one for use;
step nine: introducing chlorine into the iron chloride water phase in the fourth step to prepare an iron trichloride solution;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
In some embodiments, step one: the acid solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid.
In some embodiments, the acidic solution has a hydrogen ion concentration of 10-45mol/L, the mass ratio of the titanium chloride dust collecting slag to the acid solution is 1: 1-1: 10, and the concentration of hydrogen ions in the mixed slurry is 10-4～5mol/L。
In some embodiments, step two: concentration of hydrogen ions in the metal chloride solution 10-55mol/L, and the content of insoluble substances is not more than 2 percent.
In some embodiments, step three: and washing and filtering for multiple times until the pH value of the washed solid is 5-9 and the water content of the solid is 20-50% to obtain a first product.
In some embodiments, the product consists of the following components in percentage by mass: 20-80% of titanium oxide, 10-40% of silicon oxide and 5-60% of carbon.
In some embodiments, step four: the mass ratio of the extracting agent to the metal chloride solution is 1: 5-5: 1, and the extraction temperature is 10-95 ℃.
In some embodiments, the extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 60-99% of kerosene or sulfonated kerosene by mass percent.
In some embodiments, step four: the iron chloride water phase contains iron chloride and manganese dichloride, and the first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride.
In some embodiments, the scandium trichloride concentration is 0.1-10 g/L, the zirconium tetrachloride concentration is 1-100 g/L, the hafnium tetrachloride concentration is 0.01-5 g/L, the vanadyl dichloride concentration is 1-100 g/L, and the titanyl dichloride concentration is 1-100 g/L, wherein the mass percentages of the iron chloride and the manganese dichloride in the iron chloride aqueous phase are 8-35% of the iron chloride and 0.5-15% of the manganese dichloride.
In some embodiments, step five: the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, the mass percentage concentration of the alkali liquor is 0.01-35%, and the mass ratio of the first oil phase to the alkali liquor is 1: 10-20: 1.
In some embodiments, step five: the first alkaline solution contains scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In some embodiments, step five: the back extraction temperature is 10-100 ℃, and the back extraction time is 0.05-5 h.
In some embodiments, step six: the aging temperature is 30-180 ℃, and the aging time is 0.1-48 h.
In some embodiments, step seven: the second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
In some embodiments, step eight: adding strong acid into the second oil phase, adjusting the pH value to be 0-4 to form a new extracting agent, and adding strong acid into the second alkaline solution, adjusting the pH value to be 0-4 to form a new acidic solution.
In some embodiments, step nine: the concentration of hydrogen ions in the ferric trichloride solution is 10-4And 5mol/L, wherein the mass percent concentration of the ferric trichloride is 10-38%.
In some embodiments, step ten: and the third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 1-4, and the mass percentage concentration of the ferric aluminum chloride is 10-38%.
Compared with the prior art, the invention has the beneficial effects that: (1) different products are formed in the treated titanium chloride dust-collecting slag, so that the cyclic utilization, the reduction and the harmless treatment of resources are realized; (2) the treatment process effectively utilizes the chlorine tail gas generated in the production process of titanium dioxide by a chlorination method, and reduces the purification treatment investment of the chlorine tail gas; (3) the process can realize the treatment of the dust collecting slag only by using a small amount of alkali liquor, saves a large amount of alkali by acid-base neutralization treatment in the prior art, saves the fund, and is more environment-friendly.
Drawings
FIG. 1 is a schematic view of a titanium chloride dust-collecting slag treatment process of the invention.
Detailed Description
The present invention is described in detail with reference to the embodiments shown in the drawings, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should understand that functional, methodological, or structural equivalents or substitutions made by these embodiments are within the scope of the present invention.
Example 1
As shown in FIG. 1, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acidic solution to form a mixed slurry, wherein the acidic solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid, and hydrochloric acid is preferred in the embodiment.
The concentration of hydrogen ions in the acidic solution is 10-4mol/L, the mass ratio of the titanium chloride dust-collecting slag to the acid solution is 1:1, and the concentration of hydrogen ions in the mixed slurry is 10-4mol/L。
Step two: the mixed slurry is subjected to a filtration process to form solids including titanium dioxide, silica and carbon and a metal chloride solution. In the second step, the filtration process can be performed by using a device such as a cluster filter, a ceramic membrane filter or an organic membrane filter, and the like, in this embodiment, the cluster filter is preferably used for the filtration process, and the hydrogen ion concentration in the metal chloride solution in the second step is 10-5mol/L, and insoluble content is not more than 2%.
Step three: and (5) washing and filtering the solid in the step two for multiple times until the pH value of the washed solid is 5 and the water content of the solid is 20%, so as to obtain a product I.
The product comprises the following components in percentage by mass: 80% of titanium oxide, 10% of silicon oxide and 10% of carbon.
The aqueous solution used for washing the solid for multiple times in the step can be returned to the step one to be used as an acidic solution for replenishment.
Step four: and (4) extracting the metal chloride solution in the step two by using an extracting agent to separate an iron chloride water phase and a first oil phase.
The first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride, and the iron chloride water phase contains iron chloride and manganese dichloride.
The mass ratio of the extracting agent to the metal chloride solution is 1:5, and the extraction temperature is 10 ℃. The extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 99-60% of kerosene or sulfonated kerosene by mass percent. The extracting agent of the embodiment is preferably a kerosene and P350 mixed oily liquid, and the mass percent of the kerosene in the extracting agent is 60%.
In the fourth step, the concentration of scandium trichloride is 1g/L, the concentration of zirconium tetrachloride is 100g/L, the concentration of hafnium tetrachloride is 0.01g/L, the concentration of vanadyl dichloride is 1g/L, and the concentration of titanyl dichloride is 100g/L, wherein the mass percentages of iron chloride and manganese dichloride in the iron chloride water phase are that the iron chloride is 35% and the manganese dichloride is 0.5%.
Step five: and (3) adding the alkali liquor into the first oil phase in the fourth step, and performing back extraction to prepare a first alkaline solution containing scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In the fifth step, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, and in this embodiment, the sodium hydroxide alkali liquor is preferred. The mass percentage concentration of the alkali liquor is 0.01%, and the mass ratio of the first oil phase to the alkali liquor is 20: 1.
In the fifth step, the back extraction temperature is 10 ℃, and the back extraction time is 5 hours.
Step six: and (5) aging the first alkaline solution in the fifth step at the aging temperature of 30 ℃ for 48 h.
Step seven: and (5) centrifugally separating the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product.
The second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
Step eight: and (3) adding a strong acid into the second oil phase in the step seven, adjusting the pH value to be 0 to form a new extracting agent, returning the extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to be 0 to form a new acidic solution, and returning the new acidic solution to the step one for use.
Step nine: introducing chlorine gas into the iron chloride water phase in the fourth step to prepare ferric trichloride solution, wherein the concentration of hydrogen ions in the ferric trichloride solution is 10-4mol/L, wherein the mass percentage concentration of the ferric trichloride is 10-38%;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
The third product is an iron aluminum chloride solution, the pH value of the iron aluminum chloride solution is 1, and the mass percentage concentration of the iron aluminum chloride is 10-38%.
By the treatment process, the titanium chloride dust-collecting slag is converted into different products, and finally three products can be obtained. The main components of the product I are titanium oxide, silicon oxide and carbon, and the product I can be used as a raw material for extracting rutile, superfine silicon oxide and carbon powder; the main components of the product II are scandium oxide, zirconium oxide, sodium vanadate and hafnium oxide, and the main components can be used as raw materials for extracting scandium oxide, zirconium oxide, vanadium pentoxide and hafnium oxide; the main component of the product is ferric aluminum chloride solution, and because the solution contains aluminum ions and iron ions, aluminum hydroxide and ferric hydroxide colloid with adsorbability are formed after hydrolysis and are used as water purifying agents.
Example 2
As shown in FIG. 1, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acidic solution to form a mixed slurry, wherein the acidic solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid, and sulfuric acid is preferred in the embodiment.
The concentration of hydrogen ions in the acid solution is 1mol/L, the mass ratio of the titanium chloride dust-collecting slag to the acid solution is 1:3, and the concentration of hydrogen ions in the mixed slurry is 1 mol/L.
Step two: the mixed slurry is subjected to a filtration process to form solids including titanium dioxide, silica and carbon and a metal chloride solution. In the second step, the filtration process may be performed by using a device such as a cluster filter, a ceramic membrane filter, or an organic membrane filter, and the like, in this embodiment, the filtration process is preferably performed by using a ceramic membrane filter, and in the second step, the hydrogen ion concentration in the metal chloride solution is 1mol/L, and the content of insoluble substances is not more than 2%.
Step three: and (5) washing and filtering the solid in the step two for multiple times until the pH value of the washed solid is 6 and the water content of the solid is 20%, so as to obtain a product I.
The product comprises the following components in percentage by mass: 40% of titanium oxide, 40% of silicon oxide and 20% of carbon.
The aqueous solution used for washing the solid for multiple times in the step can be returned to the step one to be used as an acidic solution for replenishment.
Step four: and (4) extracting the metal chloride solution in the step two by using an extracting agent to separate an iron chloride water phase and a first oil phase.
The first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride, and the iron chloride water phase contains iron chloride and manganese dichloride.
The mass ratio of the extracting agent to the metal chloride solution is 1:1, and the extraction temperature is 30 ℃. The extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 99-60% of kerosene or sulfonated kerosene by mass percent. The extractant of the embodiment is preferably a sulfonated kerosene and P204 mixed oily liquid, and the mass percent of the sulfonated kerosene in the extractant is 70%.
In the fourth step, the concentration of scandium trichloride is 0.1g/L, the concentration of zirconium tetrachloride is 70g/L, the concentration of hafnium tetrachloride is 1g/L, the concentration of vanadyl dichloride is 20g/L, and the concentration of titanyl dichloride is 100g/L, wherein the mass percentages of iron chloride and manganese dichloride in the iron chloride water phase are that the iron chloride is 30% and the manganese dichloride is 8%.
Step five: and (3) adding the alkali liquor into the first oil phase in the fourth step, and performing back extraction to prepare a first alkaline solution containing scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In the fifth step, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, and in this embodiment, the sodium hydroxide alkali liquor is preferred. The mass percentage concentration of the alkali liquor is 1%, and the mass ratio of the first oil phase to the alkali liquor is 1: 1.
In the fifth step, the back extraction temperature is 20 ℃, and the back extraction time is 4.5 h.
Step six: and D, aging the first alkaline solution in the fifth step at the aging temperature of 40 ℃ for 40 h.
Step seven: and (5) centrifugally separating the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product.
The second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
Step eight: and (3) adding a strong acid into the second oil phase in the step seven, adjusting the pH value to be 1 to form a new extracting agent, returning the extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to be 1 to form a new acidic solution, and returning the new acidic solution to the step one for use.
Step nine: introducing chlorine gas into the iron chloride water phase in the fourth step to prepare an iron trichloride solution, wherein the hydrogen ion concentration of the iron trichloride solution is 1mol/L, and the mass percent concentration of the iron trichloride is 12%;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
The third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 1, and the mass percentage concentration of the ferric aluminum chloride is 15%.
By the treatment process, the titanium chloride dust-collecting slag is converted into different products, and finally three products can be obtained. The main components of the product I are titanium oxide, silicon oxide and carbon, and the product I can be used as a raw material for extracting rutile, superfine silicon oxide and carbon powder; the main components of the product II are scandium oxide, zirconium oxide, sodium vanadate and hafnium oxide, and the main components can be used as raw materials for extracting scandium oxide, zirconium oxide, vanadium pentoxide and hafnium oxide; the main component of the product is ferric aluminum chloride solution, and because the solution contains aluminum ions and iron ions, aluminum hydroxide and ferric hydroxide colloid with adsorbability are formed after hydrolysis and are used as water purifying agents.
Example 3
As shown in FIG. 1, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acidic solution to form a mixed slurry, wherein the acidic solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid, and hydrochloric acid is preferred in the embodiment.
The concentration of hydrogen ions in the acid solution is 2mol/L, the mass ratio of the titanium chloride dust-collecting slag to the acid solution is 1:4, and the concentration of hydrogen ions in the mixed slurry is 2 mol/L.
Step two: the mixed slurry is subjected to a filtration process to form solids including titanium dioxide, silica and carbon and a metal chloride solution. In the second step, the filtration process may be performed by using a device such as a cluster filter, a ceramic membrane filter, or an organic membrane filter, and the like, in this embodiment, the filtration process is preferably performed by using a ceramic membrane filter, and in the second step, the hydrogen ion concentration in the metal chloride solution is 2mol/L, and the content of insoluble substances is not more than 2%.
Step three: and (5) washing and filtering the solid in the step two for multiple times until the pH value of the washed solid is 6 and the water content of the solid is 25%, so as to obtain a product I.
The product comprises the following components in percentage by mass: 70% of titanium oxide, 25% of silicon oxide and 5% of carbon.
The aqueous solution used for washing the solid for multiple times in the step can be returned to the step one to be used as an acidic solution for replenishment.
Step four: and (4) extracting the metal chloride solution in the step two by using an extracting agent to separate an iron chloride water phase and a first oil phase.
The first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride, and the iron chloride water phase contains iron chloride and manganese dichloride.
The mass ratio of the extracting agent to the metal chloride solution is 2:1, and the extraction temperature is 50 ℃. The extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 99-60% of kerosene or sulfonated kerosene by mass percent. In the embodiment, the extracting agent is preferably a mixture of sulfonated kerosene and tributyl phosphate as oily liquid, and the mass percentage of the sulfonated kerosene in the extracting agent is 80%.
In the fourth step, the concentration of scandium trichloride is 3g/L, the concentration of zirconium tetrachloride is 50g/L, the concentration of hafnium tetrachloride is 2g/L, the concentration of vanadyl dichloride is 60g/L, and the concentration of titanyl dichloride is 80g/L, wherein the mass percentages of iron chloride and manganese dichloride in the iron chloride water phase are that the iron chloride is 26% and the manganese dichloride is 10%.
Step five: and (3) adding the alkali liquor into the first oil phase in the fourth step, and performing back extraction to prepare a first alkaline solution containing scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In the fifth step, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, and in this embodiment, the sodium hydroxide alkali liquor is preferred. The mass percentage concentration of the alkali liquor is 12%, and the mass ratio of the first oil phase to the alkali liquor is 3: 1.
In the fifth step, the back extraction temperature is 40 ℃, and the back extraction time is 3.5 h.
Step six: and (5) aging the first alkaline solution in the fifth step at the aging temperature of 50 ℃ for 35 h.
Step seven: and (5) centrifugally separating the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product.
The second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
Step eight: and (3) adding a strong acid into the second oil phase in the step seven, adjusting the pH value to be 2 to form a new extracting agent, returning the extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to be 3 to form a new acidic solution, and returning the new acidic solution to the step one for use.
Step nine: introducing chlorine gas into the iron chloride water phase in the fourth step to prepare an iron trichloride solution, wherein the concentration of hydrogen ions in the iron trichloride solution is 2mol/L, and the mass percent concentration of the iron trichloride is 18%;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
The third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 2, and the mass percentage concentration of the ferric aluminum chloride is 20%.
By the treatment process, the titanium chloride dust-collecting slag is converted into different products, and finally three products can be obtained. The main components of the product I are titanium oxide, silicon oxide and carbon, and the product I can be used as a raw material for extracting rutile, superfine silicon oxide and carbon powder; the main components of the product II are scandium oxide, zirconium oxide, sodium vanadate and hafnium oxide, and the main components can be used as raw materials for extracting scandium oxide, zirconium oxide, vanadium pentoxide and hafnium oxide; the main component of the product is ferric aluminum chloride solution, and because the solution contains aluminum ions and iron ions, aluminum hydroxide and ferric hydroxide colloid with adsorbability are formed after hydrolysis and are used as water purifying agents.
Example 4
As shown in FIG. 1, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acidic solution to form a mixed slurry, wherein the acidic solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid, and hydrochloric acid is preferred in the embodiment.
The concentration of hydrogen ions in the acid solution is 4mol/L, the mass ratio of the titanium chloride dust-collecting slag to the acid solution is 1:6, and the concentration of hydrogen ions in the mixed slurry is 4 mol/L.
Step two: the mixed slurry is subjected to a filtration process to form solids including titanium dioxide, silica and carbon and a metal chloride solution. In the second step, the filtration process can be carried out by using a device such as a cluster filter, a ceramic membrane filter or an organic membrane filter, and the like, in this embodiment, the filtration process is preferably carried out by using an organic membrane filter, and in the second step, the hydrogen ion concentration in the metal chloride solution is 4mol/L, and the content of insoluble substances is not more than 2%.
Step three: and (5) washing and filtering the solid in the step two for multiple times until the pH value of the washed solid is 7 and the water content of the solid is 30%, so as to obtain a product I.
The product comprises the following components in percentage by mass: 50% of titanium oxide, 30% of silicon oxide and 20% of carbon.
The aqueous solution used for washing the solid for multiple times in the step can be returned to the step one to be used as an acidic solution for replenishment.
Step four: and (4) extracting the metal chloride solution in the step two by using an extracting agent to separate an iron chloride water phase and a first oil phase.
The first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride, and the iron chloride water phase contains iron chloride and manganese dichloride.
The mass ratio of the extracting agent to the metal chloride solution is 4:1, and the extraction temperature is 70 ℃. The extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 99-60% of kerosene or sulfonated kerosene by mass percent. In the embodiment, the extracting agent is preferably a kerosene and tributyl phosphate mixed oily liquid, and the mass percent of the kerosene in the extracting agent is 90%.
In the fourth step, the concentration of scandium trichloride is 7g/L, the concentration of zirconium tetrachloride is 20g/L, the concentration of hafnium tetrachloride is 4g/L, the concentration of vanadyl dichloride is 100g/L, and the concentration of titanyl dichloride is 10g/L, wherein the mass percentages of iron chloride and manganese dichloride in the iron chloride water phase are that the iron chloride is 30% and the manganese dichloride is 12%.
Step five: and (3) adding the alkali liquor into the first oil phase in the fourth step, and performing back extraction to prepare a first alkaline solution containing scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In the fifth step, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, and in this embodiment, the sodium hydroxide alkali liquor is preferred. The mass percentage concentration of the alkali liquor is 30%, and the mass ratio of the first oil phase to the alkali liquor is 10: 1.
In the fifth step, the back extraction temperature is 70 ℃, and the back extraction time is 2 hours.
Step six: and (5) aging the first alkaline solution in the fifth step at the aging temperature of 130 ℃ for 8 h.
Step seven: and (5) centrifugally separating the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product.
The second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
Step eight: and (3) adding a strong acid into the second oil phase in the step seven, adjusting the pH value to be 4 to form a new extracting agent, returning the extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to be 3 to form a new acidic solution, and returning the new acidic solution to the step one for use.
Step nine: introducing chlorine gas into the iron chloride water phase in the fourth step to prepare an iron trichloride solution, wherein the hydrogen ion concentration of the iron trichloride solution is 4mol/L, and the mass percent concentration of the iron trichloride is 30%;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
The third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 3, and the mass percentage concentration of the ferric aluminum chloride is 30%.
By the treatment process, the titanium chloride dust-collecting slag is converted into different products, and finally three products can be obtained. The main components of the product I are titanium oxide, silicon oxide and carbon, and the product I can be used as a raw material for extracting rutile, superfine silicon oxide and carbon powder; the main components of the product II are scandium oxide, zirconium oxide, sodium vanadate and hafnium oxide, and the main components can be used as raw materials for extracting scandium oxide, zirconium oxide, vanadium pentoxide and hafnium oxide; the main component of the product is ferric aluminum chloride solution, and because the solution contains aluminum ions and iron ions, aluminum hydroxide and ferric hydroxide colloid with adsorbability are formed after hydrolysis and are used as water purifying agents.
Example 5
As shown in FIG. 1, the invention provides a titanium chloride dust-collecting slag treatment process, which comprises the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acidic solution to form a mixed slurry, wherein the acidic solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid, and hydrochloric acid is preferred in the embodiment.
The concentration of hydrogen ions in the acid solution is 5mol/L, the mass ratio of the titanium chloride dust-collecting slag to the acid solution is 1:10, and the concentration of hydrogen ions in the mixed slurry is 5 mol/L.
Step two: the mixed slurry is subjected to a filtration process to form solids including titanium dioxide, silica and carbon and a metal chloride solution. In the second step, the filtration process can be carried out by using a device such as a cluster filter, a ceramic membrane filter or an organic membrane filter, and the like, in this embodiment, the filtration process is preferably carried out by using an organic membrane filter, and in the second step, the hydrogen ion concentration in the metal chloride solution is 5mol/L, and the content of insoluble substances is not more than 2%.
Step three: and (5) washing and filtering the solid in the step two for multiple times until the pH value of the washed solid is 9 and the water content of the solid is 50%, so as to obtain a product I.
The product comprises the following components in percentage by mass: 20% of titanium oxide, 20% of silicon oxide and 60% of carbon.
The aqueous solution used for washing the solid for multiple times in the step can be returned to the step one to be used as an acidic solution for replenishment.
Step four: and (4) extracting the metal chloride solution in the step two by using an extracting agent to separate an iron chloride water phase and a first oil phase.
The first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride, and the iron chloride water phase contains iron chloride and manganese dichloride.
The mass ratio of the extracting agent to the metal chloride solution is 5:1, and the extraction temperature is 95 ℃. The extracting agent is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extracting agent contains 99-60% of kerosene or sulfonated kerosene by mass percent. The extracting agent of the embodiment is preferably a kerosene and P350 mixed oily liquid, and the mass percent of the kerosene in the extracting agent is 99%.
In the fourth step, the concentration of scandium trichloride is 10g/L, the concentration of zirconium tetrachloride is 1g/L, the concentration of hafnium tetrachloride is 5g/L, the concentration of vanadyl dichloride is 1g/L, and the concentration of titanyl dichloride is 100g/L, wherein the mass percentages of iron chloride and manganese dichloride in the iron chloride water phase are that the iron chloride is 35% and the manganese dichloride is 15%.
Step five: and (3) adding the alkali liquor into the first oil phase in the fourth step, and performing back extraction to prepare a first alkaline solution containing scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
In the fifth step, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, and in this embodiment, the sodium hydroxide alkali liquor is preferred. The mass percentage concentration of the alkali liquor is 35%, and the mass ratio of the first oil phase to the alkali liquor is 20: 1.
In the fifth step, the back extraction temperature is 100 ℃, and the back extraction time is 0.05 h.
Step six: and (5) aging the first alkaline solution in the fifth step at 180 ℃ for 0.1 h.
Step seven: and (5) centrifugally separating the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product.
The second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
Step eight: and (3) adding a strong acid into the second oil phase in the step seven, adjusting the pH value to be 4 to form a new extracting agent, returning the extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to be 4 to form a new acidic solution, and returning the new acidic solution to the step one for use.
Step nine: introducing chlorine into the iron chloride water phase in the fourth step to prepare an iron trichloride solution, wherein the hydrogen ion concentration of the iron trichloride solution is 5mol/L, and the mass percent concentration of the iron trichloride is 38%;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
The third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 4, and the mass percentage concentration of the ferric aluminum chloride is 38%.
By the treatment process, the titanium chloride dust-collecting slag is converted into different products, and finally three products can be obtained. The main components of the product I are titanium oxide, silicon oxide and carbon, and the product I can be used as a raw material for extracting rutile, superfine silicon oxide and carbon powder; the main components of the product II are scandium oxide, zirconium oxide, sodium vanadate and hafnium oxide, and the main components can be used as raw materials for extracting scandium oxide, zirconium oxide, vanadium pentoxide and hafnium oxide; the main component of the product is ferric aluminum chloride solution, and because the solution contains aluminum ions and iron ions, aluminum hydroxide and ferric hydroxide colloid with adsorbability are formed after hydrolysis and are used as water purifying agents.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (18)

1. The titanium chloride dust-collecting slag treatment process is characterized by comprising the following steps:
the method comprises the following steps: mixing and dissolving titanium chloride dust-collecting slag and an acid solution to form mixed slurry;
step two: filtering the mixed slurry to form solids and a metal chloride solution, wherein the solids comprise titanium dioxide, silicon dioxide and carbon;
step three: washing and filtering the solid in the step two for multiple times to obtain a product I;
step four: extracting the metal chloride solution in the step two to separate an iron chloride water phase and a first oil phase;
step five: adding alkali liquor into the first oil phase in the fourth step, and preparing a first alkaline solution through back extraction;
step six: aging the first alkaline solution in the fifth step;
step seven: centrifuging the first alkaline solution in the sixth step to obtain a second oil phase, a second alkaline solution and a second product;
step eight: adding a strong acid into the second oil phase in the step seven, adjusting the pH value to form a new extracting agent, returning the new extracting agent to the step four for use, adding a strong acid into the second alkaline solution, adjusting the pH value to form a new acidic solution, and returning the new acidic solution to the step one for use;
step nine: introducing chlorine into the iron chloride water phase in the fourth step to prepare an iron trichloride solution;
step ten: and (4) adding aluminum hydroxide into the ferric trichloride solution in the step nine to prepare a product III.
2. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the following steps: the acid solution is hydrochloric acid or sulfuric acid or a mixed solution of hydrochloric acid and sulfuric acid.
3. The titanium chloride dust collecting slag treatment process according to claim 2, wherein the concentration of hydrogen ions in the acidic solution is 10-45mol/L, the mass ratio of the titanium chloride dust collecting slag to the acid solution is 1: 1-1: 10, and the concentration of hydrogen ions in the mixed slurry is 10-4～5mol/L。
4. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the following steps: concentration of hydrogen ions in the metal chloride solution 10-55mol/L, and the content of insoluble substances is not more than 2 percent.
5. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the third step of: and washing and filtering for multiple times until the pH value of the washed solid is 5-9 and the water content of the solid is 20-50% to obtain a first product.
6. The titanium chloride dust collecting slag treatment process according to claim 5, wherein the product consists of the following components in percentage by mass: 20-80% of titanium oxide, 10-40% of silicon oxide and 5-60% of carbon.
7. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the fourth step of: the mass ratio of the extracting agent to the metal chloride solution is 1: 5-5: 1, and the extraction temperature is 10-95 ℃.
8. The titanium chloride dust collecting slag treatment process according to claim 7, wherein the extractant is a mixed oily liquid of kerosene or sulfonated kerosene and P204 or P350 or tributyl phosphate, and the extractant contains 60-99% of kerosene or sulfonated kerosene by mass percent.
9. The titanium chloride dust collecting slag treatment process according to claim 8, characterized by comprising the fourth step of: the iron chloride water phase contains iron chloride and manganese dichloride, and the first oil phase contains scandium trichloride, zirconium tetrachloride, hafnium tetrachloride, vanadyl dichloride and titanyl dichloride.
10. The titanium chloride dust-collecting slag treatment process according to claim 9, wherein the scandium chloride is 0.1-10 g/L in concentration, the zirconium tetrachloride is 1-100 g/L in concentration, the hafnium tetrachloride is 0.01-5 g/L in concentration, the vanadyl dichloride is 1-100 g/L in concentration, and the titanyl dichloride is 1-100 g/L in concentration, and the mass percentages of the iron chloride and the manganese dichloride in the iron chloride aqueous phase are 8-35% of the iron chloride and 0.5-15% of the manganese dichloride.
11. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the following five steps: the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, the mass percentage concentration of the alkali liquor is 0.01-35%, and the mass ratio of the first oil phase to the alkali liquor is 1: 10-20: 1.
12. The titanium chloride dust collecting slag treatment process according to claim 11, characterized by comprising the following five steps: the first alkaline solution contains scandium hydroxide, zirconium hydroxide, sodium vanadate and hafnium hydroxide.
13. The titanium chloride dust collecting slag treatment process according to claim 12, characterized by comprising the following five steps: the back extraction temperature is 10-100 ℃, and the back extraction time is 0.05-5 h.
14. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the sixth step of: the aging temperature is 30-180 ℃, and the aging time is 0.1-48 h.
15. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the seventh step of: the second product comprises the following components in percentage by mass: 0.5-30% of scandium oxide, 5-30% of zirconium oxide, 0.5-10% of sodium vanadate and 1-5% of hafnium oxide.
16. The titanium chloride dust collecting slag treatment process according to claim 15, characterized by comprising the following eight steps: adding strong acid into the second oil phase, adjusting the pH value to be 0-4 to form a new extracting agent, and adding strong acid into the second alkaline solution, adjusting the pH value to be 0-4 to form a new acidic solution.
17. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the nine steps of: the concentration of hydrogen ions in the ferric trichloride solution is 10-4And 5mol/L, wherein the mass percent concentration of the ferric trichloride is 10-38%.
18. The titanium chloride dust collecting slag treatment process according to claim 1, characterized by comprising the following ten steps: and the third product is ferric aluminum chloride solution, the pH value of the ferric aluminum chloride solution is 1-4, and the mass percentage concentration of the ferric aluminum chloride is 10-38%.
CN202011351807.1A 2020-11-27 2020-11-27 Titanium chloride dust collection slag treatment process Pending CN112609075A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104178632A (en) * 2014-08-12 2014-12-03 东北大学 Method for comprehensively utilizing titanium white waste acid
CN105836862A (en) * 2016-04-01 2016-08-10 郑州轻工业学院 Comprehensive treatment method for recovery dust produced in production of titanium tetrachloride through boiling chlorination
CN106629810A (en) * 2016-12-30 2017-05-10 锦州海特新材料科技有限公司 Method for preparing scandium oxide via chlorinated soot

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104178632A (en) * 2014-08-12 2014-12-03 东北大学 Method for comprehensively utilizing titanium white waste acid
CN105836862A (en) * 2016-04-01 2016-08-10 郑州轻工业学院 Comprehensive treatment method for recovery dust produced in production of titanium tetrachloride through boiling chlorination
CN106629810A (en) * 2016-12-30 2017-05-10 锦州海特新材料科技有限公司 Method for preparing scandium oxide via chlorinated soot

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