CN101994012A - Method for producing titanium dioxide by using titanium-containing blast furnace slag - Google Patents
Method for producing titanium dioxide by using titanium-containing blast furnace slag Download PDFInfo
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- CN101994012A CN101994012A CN2010105762060A CN201010576206A CN101994012A CN 101994012 A CN101994012 A CN 101994012A CN 2010105762060 A CN2010105762060 A CN 2010105762060A CN 201010576206 A CN201010576206 A CN 201010576206A CN 101994012 A CN101994012 A CN 101994012A
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Abstract
The invention relates to a comprehensive utilization technology of blast furnace slag, in particular to a method for producing titanium dioxide by using titanium-containing blast furnace slag. The technical scheme comprises the following steps of: crushing, ball milling and screening titanium-bearing blast furnace slag, and placing in a molten salt system containing NaOH and NaNO3; washing the intermediate product in water at 60-75 DEG C, and filtering; removing impurities of a NaOH and NaNO3 alkaline solution containing sodium silicate and sodium metaaluminate, concentrating, and returning to the NaOH and NaNO3 molten salt system; dissolving the washing material containing solid phase sodium titanate by using an inorganic acid, adding a reducing agent for a reduction reaction, and then filtering; filtering the titanium-containing solution to obtain an inorganic acid filtrate and a metatitanic acid product; and calcining the metatitanic acid product at 600-1300 DEG C to obtain the final product of titanium dioxide powder. The invention realizes high conversion rate of titanium, and furthest reduces environmental pollution at the same time.
Description
Technical field
The present invention relates to a kind of comprehensive utilization technique of blast furnace slag, be specifically related to a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide.
Background technology
China's v-ti magnetite ore reserves is bigger, and having verified is 61.9 hundred million tons.At present, China has at first solved the technical barrier that utilizes blast-furnace smelting high titanium type iron (vanadium) concentrate to produce the pig iron, but most of titaniferous thing is then deposited slag mutually with very tiny the tax with the dispersive state mutually, become and contain 15 ~ 25% titanium-containing blast furnace slag, uhligite in the titanium-containing blast furnace slag is compared stable, and activity is lower, is difficult to handle, the titanium-containing blast furnace slag of bulk deposition has caused the loss of titanium resource, and environment has also been caused huge pollution.At present, for from addressing the above problem, the scientific worker has carried out a large amount of work, can be divided into following three classes:
The first kind: the master alloy technology, mainly adopt silicothermic process reduction+electrosmelting ferro-titanium technology.Though this method can be utilized part titanium in the titanium-containing blast furnace slag, current consumption is big, and cost is higher, and treatment scale is limited.
Second class: carbonization, chlorination technique, mainly adopt high temperature cabonization-low temperature chlorination producing titanium tetrachloride t 5 bx technology, high temperature cabonization-carbide slag sorting titanium carbide technology.The rate of recovery of such carbonization, chlorination technique titanium is higher, but the processing condition harshness, treatment capacity is limited, and the muriate residue of a large amount of by-products is difficult to digestion, serious environment pollution.
The 3rd class: wet chemistry method mainly contains acid system and produces the titanium dioxide technology.Though this method is easy to operate, technology is simple, no matter be that sulfuric acid process or salt acid system are carried titanium, all there is the problem that spent acid is difficult to utilize after the hydrolysis, also can cause secondary pollution.As Cao Hongyang, pay new the grade in the document of delivering that is called " the hydrochloric acid pressurization leaching of modified titanium-containing furnace cinder " of thought the method for utilizing hydrochloric acid that the titanium in the high filter residue is leached under condition of high voltage has been described.
Although such scheme is technical feasible,, finally fail to realize resource utilization, the eco-utilization of titanium-containing blast furnace slag owing to still have problems such as secondary pollution, energy consumption is big, treatment capacity is little.
Summary of the invention
The objective of the invention is deficiency, a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide is provided, in the high conversion of realizing titanium, reduce pollution the biglyyest environment at the prior art existence.
The technical scheme that realizes the object of the invention is to carry out according to the following steps:
(1) with titanium-containing blast furnace slag after broken, ball milling and screening, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH in the molten salt system and titanium-containing blast furnace slag is 1 ~ 10:1, NaOH and NaNO
3Mol ratio be 1 ~ 10:1, temperature be under 200 ~ 700 ℃ of conditions the reaction 3 hours, the acquisition main component is the intermediate product of sodium titanate, water glass and sodium metaaluminate;
(2) then above-mentioned intermediate product is washed after-filtration in 60 ~ 75 ℃ water, soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) will contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye return described NaOH and NaNO through removal of impurities, after concentrating
3In the molten salt system, water glass and sodium metaaluminate are as the raw material of producing aluminium byproduct and silicon byproduct;
(4) after the washing material that contains the solid phase sodium titanate dissolves with mineral acid, add reductive agent and carry out the reduction reaction after-filtration, filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate after 1 ~ 20 hour, more after filtration, obtains mineral acid filtrate and metatitanic acid product 40 ~ 110 ℃ of following hydrolysis; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product obtains the finished product titanium dioxide powder 600 ~ 1300 ℃ of calcinings down.
Titanium elements mainly exists with the form of uhligite phase in the described titanium-containing blast furnace slag, and the weight percent of titanium is 10 ~ 50%.
The ball milling time in the described step (1) is 24 ~ 72h, and the titanium-containing blast furnace slag behind the ball milling sieves through 200 mesh standard sieves.
Described titanium-containing blast furnace slag after fragmentation, ball milling and screening places and contains NaOH and NaNO
3Molten salt system in, the leaching yield of titanium reaches more than 70%;
Solid-liquid mass ratio when washing with water in the described step (2) is 1:20 ~ 40.
It is 5% hydrochloric acid soln that described mineral acid is selected volumetric concentration for use.
Described reductive agent is selected S-WAT for use.
Described the finished product titanium dioxide powder is a rutile titanium dioxide, quality purity〉97.6%.
Compare with technology with existing, characteristics of the present invention and beneficial effect thereof are:
(1) the present invention proposes employing NaOH+ NaNO
3Molten salt system is handled titanium-containing blast furnace slag, compares with roasting method with traditional chlorination process and has reduced about 400 ℃ of temperature of reaction, has not only reduced energy consumption, and technical difficulty and facility investment expense significantly reduce, and has improved the operability of technology.
(2) the present invention uses titanium-containing blast furnace slag to be raw material, owing to need not condition of high voltage, has reduced the requirement to equipment with pressurization salt acid system comparison in the document, and the NaOH+ NaNO that recycles of the present invention
3Molten salt system has been avoided the secondary pollution of using hydrochloric acid that environment is caused when reducing production costs;
(3) decomposition media is carried out internal recycling in the technical solution of the present invention, acid circulates and isolation technique greatly reduces production energy consumption, and the minimizing of bed drain purge, and the no dust discharge of waste gas has been avoided environmental pollution.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is the SEM figure of the prepared titanium dioxide of the embodiment of the invention 1.
Fig. 3 is the XRD figure of the prepared titanium dioxide of the embodiment of the invention 1.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment:
Embodiment 1:
(1) with titanium-containing blast furnace slag through broken, ball milling 24 hours with after being sized to 200 orders, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH and titanium-containing blast furnace slag is 4:1, NaOH and NaNO
3Mol ratio be 4:1, temperature be under 500 ℃ of conditions the reaction 3 hours, the acquisition composition is the intermediate product of sodium titanate, water glass and sodium metaaluminate, the leaching yield of titanium reaches more than 72.5%;
(2) then above-mentioned intermediate product is washed also filter 23 in 60 ℃ water, wash the solid-liquid mass ratio is 1:20 at every turn, and soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye returns the NaOH and the NaNO of step (1) through removal of impurities, after concentrating
3Molten salt system, impurity is as the raw material of producing aluminium byproduct and silicon byproduct;
(4) the washing material volumetric concentration that contains the solid phase sodium titanate is after 5% hydrochloric acid dissolves, to add Sodium Nitrite and carry out the reduction reaction after-filtration, and filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate is 85 ℃ of following hydrolysis after 6 hours in temperature, more after filtration, obtains mineral acid filtrate and metatitanic acid product; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product is 650 ℃ of down calcinings 6 hours in temperature, and obtaining the finished product is rutile titanium dioxide, its SEM figure as shown in Figure 2, its XRD spectra as shown in Figure 3, titanium dioxide purity is 97.6%.
Embodiment 2:
(1) with titanium-containing blast furnace slag through broken, ball milling 36 hours with after being sized to 200 orders, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH and titanium-containing blast furnace slag is 3:1, NaOH and NaNO
3Mol ratio be 3:1, temperature be under 450 ℃ of conditions the reaction 3 hours, the acquisition composition is the intermediate product of sodium titanate, water glass and sodium metaaluminate, the leaching yield of titanium reaches more than 70.5%;
(2) then above-mentioned intermediate product is washed also filter 23 in 60 ℃ water, wash the solid-liquid mass ratio is 1:40 at every turn, and soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye returns the NaOH and the NaNO of step (1) through removal of impurities, after concentrating
3Molten salt system, impurity is as the raw material of producing aluminium byproduct and silicon byproduct;
(4) the washing material volumetric concentration that contains the solid phase sodium titanate is after 5% hydrochloric acid dissolves, to add Sodium Nitrite and carry out the reduction reaction after-filtration, and filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate is 90 ℃ of following hydrolysis after 5 hours in temperature, more after filtration, obtains mineral acid filtrate and metatitanic acid product; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product was calcined 6 hours under temperature is 650 ℃, and obtaining the finished product is rutile titanium dioxide, and titanium dioxide purity is 98.2%.
Embodiment 3:
(1) with titanium-containing blast furnace slag through broken, ball milling 72 hours with after being sized to 200 orders, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH and titanium-containing blast furnace slag is 5:1, NaOH and NaNO
3Mol ratio be 5:1, temperature be under 550 ℃ of conditions the reaction 3 hours, the acquisition composition is the intermediate product of sodium titanate, water glass and sodium metaaluminate, the leaching yield of titanium reaches more than 73.8%;
(2) then above-mentioned intermediate product is washed also filter 23 in 70 ℃ water, wash the solid-liquid mass ratio is 1:30 at every turn, and soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye returns the NaOH and the NaNO of step (1) through removal of impurities, after concentrating
3Molten salt system, impurity is as the raw material of producing aluminium byproduct and silicon byproduct;
(4) the washing material volumetric concentration that contains the solid phase sodium titanate is after 5% hydrochloric acid dissolves, to add Sodium Nitrite and carry out the reduction reaction after-filtration, and filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate is 95 ℃ of following hydrolysis after 6 hours in temperature, more after filtration, obtains mineral acid filtrate and metatitanic acid product; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product was calcined 6 hours under temperature is 650 ℃, and obtaining the finished product is rutile titanium dioxide, and titanium dioxide purity is 98.6%.
Embodiment 4:
(1) with titanium-containing blast furnace slag through broken, ball milling 36 hours with after being sized to 200 orders, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH and titanium-containing blast furnace slag is 6:1, NaOH and NaNO
3Mol ratio be 6:1, temperature be under 600 ℃ of conditions the reaction 3 hours, the acquisition composition is the intermediate product of sodium titanate, water glass and sodium metaaluminate, the leaching yield of titanium reaches more than 75.5%;
(2) then above-mentioned intermediate product is washed in 75 ℃ water and filter 23 time, wash the solid-liquid mass ratio is 1:35 at every turn, and soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye returns the NaOH and the NaNO of step (1) through removal of impurities, after concentrating
3Molten salt system, impurity is as the raw material of producing aluminium byproduct and silicon byproduct;
(4) the washing material volumetric concentration that contains the solid phase sodium titanate is after 5% hydrochloric acid dissolves, to add Sodium Nitrite and carry out the reduction reaction after-filtration, and filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate is 80 ℃ of following hydrolysis after 6 hours in temperature, more after filtration, obtains mineral acid filtrate and metatitanic acid product; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product was calcined 6 hours under temperature is 650 ℃, and obtaining the finished product is rutile titanium dioxide, and titanium dioxide purity is 97.9%.
Claims (8)
1. method of utilizing titanium-containing blast furnace slag to produce titanium dioxide is characterized in that carrying out according to the following steps:
(1) with titanium-containing blast furnace slag after broken, ball milling and screening, place and contain NaOH and NaNO
3Molten salt system in, wherein the mass ratio of NaOH in the molten salt system and titanium-containing blast furnace slag is 1 ~ 10:1, NaOH and NaNO
3Mol ratio be 1 ~ 10:1, temperature be under 200 ~ 700 ℃ of conditions the reaction 3 hours, the acquisition main component is the intermediate product of sodium titanate, water glass and sodium metaaluminate;
(2) then above-mentioned intermediate product is washed after-filtration in 60 ~ 75 ℃ water, soluble water glass and sodium metaaluminate enter and contain NaOH and NaNO
3Alkali lye, the solid phase sodium titanate forms the washing material;
(3) will contain the NaOH and the NaNO of water glass and sodium metaaluminate
3Alkali lye return described NaOH and NaNO through removal of impurities, after concentrating
3In the molten salt system, water glass and sodium metaaluminate are as the raw material of producing aluminium byproduct and silicon byproduct;
(4) after the washing material that contains the solid phase sodium titanate dissolves with mineral acid, add reductive agent and carry out the reduction reaction after-filtration, filter residue is as cement raw material, and filtrate is titaniferous solution;
(5) above-mentioned titaniferous solution is filtered, filtrate after 1 ~ 20 hour, more after filtration, obtains mineral acid filtrate and metatitanic acid product 40 ~ 110 ℃ of following hydrolysis; Mineral acid filtrate turns back to step (4) recycle;
(6) above-mentioned metatitanic acid product obtains the finished product titanium dioxide powder 600 ~ 1300 ℃ of calcinings down.
2. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that titanium elements mainly exists with the form of uhligite phase in the described titanium-containing blast furnace slag, and the weight percent of titanium is 10 ~ 50%.
3. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that the ball milling time in the described step (1) is 24 ~ 72h, and the titanium-containing blast furnace slag behind the ball milling sieves through 200 mesh standard sieves.
4. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that described titanium-containing blast furnace slag after fragmentation, ball milling and screening, places and contains NaOH and NaNO
3Molten salt system in, the leaching yield of titanium reaches more than 70%.
5. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1, the solid-liquid mass ratio when it is characterized in that washing with water in the described step (2) is 1:20 ~ 40.
6. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that it is 5% hydrochloric acid soln that described mineral acid is selected volumetric concentration for use.
7. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that described reductive agent selects S-WAT for use.
8. a kind of method of utilizing titanium-containing blast furnace slag to produce titanium dioxide according to claim 1 is characterized in that described the finished product titanium dioxide powder is a rutile titanium dioxide, quality purity〉97.6%.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212707A (en) * | 2011-06-02 | 2011-10-12 | 东北大学 | Method for decomposing titanium-containing blast-furnace slag through fused salt |
| CN102583515A (en) * | 2012-01-09 | 2012-07-18 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN103276207A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium solution by wet-processing on vanadium-titanium magnetite concentrates |
| CN103950976A (en) * | 2014-04-04 | 2014-07-30 | 中国科学院过程工程研究所 | Method for preparing titanium dioxide by utilizing mixed alkali of sodium hydroxide and sodium nitrate |
| CN105967231A (en) * | 2016-06-22 | 2016-09-28 | 中国神华能源股份有限公司 | Method for extracting TiO2 from white clay |
| CN106277048A (en) * | 2016-08-24 | 2017-01-04 | 西南化工研究设计院有限公司 | A kind of titanium slag is utilized to prepare the method and system of anatase titanium dioxide for raw material |
| CN106564945A (en) * | 2016-10-26 | 2017-04-19 | 四川省高能钛坦环保科技有限公司 | Method for extracting titanium dioxide from blast furnace slag |
| CN106745229A (en) * | 2017-02-02 | 2017-05-31 | 罗文凤 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
| CN106795586A (en) * | 2014-07-08 | 2017-05-31 | 阿瓦塔纳有限公司 | Product is extracted from titaniferous ore |
| CN106987944A (en) * | 2017-02-26 | 2017-07-28 | 浙江峰赫纺织有限公司 | Sun-proof anti-bacterial fibre mixed yarn |
| CN112919529A (en) * | 2021-03-31 | 2021-06-08 | 成渝钒钛科技有限公司 | Method for preparing barium titanate by utilizing titanium-containing blast furnace slag |
| CN113120911A (en) * | 2021-04-20 | 2021-07-16 | 昆明理工大学 | Method for separating silicon and iron in copper smelting slag through ultrasonic enhancement and preparing white carbon black by using silicon |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212707A (en) * | 2011-06-02 | 2011-10-12 | 东北大学 | Method for decomposing titanium-containing blast-furnace slag through fused salt |
| CN102583515A (en) * | 2012-01-09 | 2012-07-18 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN102583515B (en) * | 2012-01-09 | 2014-04-02 | 安徽工业大学 | Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag |
| CN103276207A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院过程工程研究所 | Method for preparing titanium solution by wet-processing on vanadium-titanium magnetite concentrates |
| CN103276207B (en) * | 2013-05-17 | 2015-02-18 | 中国科学院过程工程研究所 | Method for preparing titanium solution by wet-processing on vanadium-titanium magnetite concentrates |
| CN103950976A (en) * | 2014-04-04 | 2014-07-30 | 中国科学院过程工程研究所 | Method for preparing titanium dioxide by utilizing mixed alkali of sodium hydroxide and sodium nitrate |
| CN106795586A (en) * | 2014-07-08 | 2017-05-31 | 阿瓦塔纳有限公司 | Product is extracted from titaniferous ore |
| US10287176B2 (en) | 2014-07-08 | 2019-05-14 | Avertana Limited | Extraction of products from titanium-bearing minerals |
| US10407316B2 (en) | 2014-07-08 | 2019-09-10 | Avertana Limited | Extraction of products from titanium-bearing minerals |
| US10294117B2 (en) | 2014-07-08 | 2019-05-21 | Avertana Limited | Extraction of products from titanium-bearing minerals |
| CN105967231A (en) * | 2016-06-22 | 2016-09-28 | 中国神华能源股份有限公司 | Method for extracting TiO2 from white clay |
| CN106277048A (en) * | 2016-08-24 | 2017-01-04 | 西南化工研究设计院有限公司 | A kind of titanium slag is utilized to prepare the method and system of anatase titanium dioxide for raw material |
| CN106564945A (en) * | 2016-10-26 | 2017-04-19 | 四川省高能钛坦环保科技有限公司 | Method for extracting titanium dioxide from blast furnace slag |
| CN106745229B (en) * | 2017-02-02 | 2018-07-31 | 徐州钛白化工有限责任公司 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
| CN106745229A (en) * | 2017-02-02 | 2017-05-31 | 罗文凤 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
| CN106987944A (en) * | 2017-02-26 | 2017-07-28 | 浙江峰赫纺织有限公司 | Sun-proof anti-bacterial fibre mixed yarn |
| CN106987944B (en) * | 2017-02-26 | 2019-03-05 | 浙江峰赫纺织有限公司 | Sun-proof anti-bacterial fibre mixed yarn |
| CN112919529A (en) * | 2021-03-31 | 2021-06-08 | 成渝钒钛科技有限公司 | Method for preparing barium titanate by utilizing titanium-containing blast furnace slag |
| CN113120911A (en) * | 2021-04-20 | 2021-07-16 | 昆明理工大学 | Method for separating silicon and iron in copper smelting slag through ultrasonic enhancement and preparing white carbon black by using silicon |
| CN113120911B (en) * | 2021-04-20 | 2023-09-12 | 昆明理工大学 | Method for ultrasonically reinforcing and separating silicon and iron in copper smelting slag and preparing white carbon black by utilizing silicon |
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