CN1793391A - Process for mfg., enriched titanium material by electric furnace titanium slag - Google Patents
Process for mfg., enriched titanium material by electric furnace titanium slag Download PDFInfo
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- CN1793391A CN1793391A CN 200510048754 CN200510048754A CN1793391A CN 1793391 A CN1793391 A CN 1793391A CN 200510048754 CN200510048754 CN 200510048754 CN 200510048754 A CN200510048754 A CN 200510048754A CN 1793391 A CN1793391 A CN 1793391A
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Abstract
The invention discloses a technology method used electric furnace titanium slag to manufacture rich titanium material. It uses TiO<SUB>2</SUB>80-87% titanium slag to manufacture rich titanium material with much than 90% TiO<SUB>2</SUB>. Its core technique is adopted autoclaving to destroy high temperature solid molten mass structure of electric furnace titanium slag, and used atmospheric pressure to leach out impurity, and finally washed out reacted derelict.
Description
Technical field: the present invention relates to a kind of TiO of utilization
280 ~ 87% titanium slags are produced TiO
2The processing method of 〉=90% rich titanium material.
Background technology: at present the method for industrial production titanium dioxide has two kinds of sulfuric acid process and chlorination processs.Wherein, sulfuric acid process starts from the twenties in last century, is used for producing the history that anatase thpe white powder had more than 60 year so far from nineteen twenty-three.Chlorination process is a kind of advanced method, comes across the end of the fifties in last century, is used to produce Rutile type Titanium Dioxide in 1958.Sulfuric acid process is a raw material with ilmenite or titanium slag, and the waste water and the refuse of discharge are many; Chlorination process is generally used the rich titanium material of higher-grade, and the waste water and the refuse of discharge are less, thereby chloride process titanium dioxide throughput increases rapidly, and the large-scale titanium powder plant that has abroad built up since the nineties in last century adopts chlorination process mostly.Along with the development of chloride process titanium dioxide powder industry, growing in recent years to the demand of the rich titanium material of higher-grade.
The product that ilmenite is produced with electric furnace smelting process is a titanium slag, usually TiO
2The product of content 〉=90% is called rich titanium material, TiO
2The product of content＜90% is called titanium slag.The product that ilmenite is produced with other method is an artificial rutile.The rich titanium material general reference of higher-grade TiO
2Rich titanium material of the electric furnace of content 〉=90% and artificial rutile.
Low (the TiO of grade at ilmenite concentrate
247 ~ 49%), the use high power electric furnace can only output TiO
2The problem of content 85 ~ 87% titanium slags.Because the low or non-iron contamination height of ilmenite concentrate grade, the titanium slag TiO that melts out with high power electric furnace
2Content do not reach 〉=90% requirement, must adopt to contain TiO
2〉=90% artificial rutile batching.
Summary of the invention: the objective of the invention is to overcome the prior art deficiency, invent a kind of electro-titanium slag that grade is lower and make TiO
2〉=90% rich titanium material is produced titanium dioxide for chlorination process and is supplied raw materials, and guarantees the quality product and the technico-economical comparison of chlorination process production titanium white from raw material; Technology of the present invention can not need with the artificial rutile batching, thereby forms ilmenite concentrate → electro-titanium slag → rich titanium material → chloride process titanium dioxide powder production technique, accomplishes environmental friendliness, utilization of resources maximization and and harmonious development from technology.
The conventional art principle: the temperature of electric furnace reduction melting is between 1500 ~ 2000 ℃, can only remove de-iron with the electrosmelting ilmenite concentrate, remaining iron and other impurity, in the crystallisation by cooling process after the titanium slag melt is come out of the stove, all impurity and part titanyl compound form anosovite Solid solution, column foot stone Solid solution and silicate glass body.The material composition of titanium slag is highly stable, and general processing condition are difficult to decompose.In sulfuric acid process, titanium slag be under high temperature, high pressure, peracid condition by acidolysis, the acidolysis rate of titanium slag requires to reach more than 94%, makes TiO
2Hydrolysis again after the dissolving, precipitation are separated out, and utilize the solubility of impurity that impurity is trapped in the solution and remove.
Theory of the present invention is opposite, at first uses the Solid solution structure of reagent selective destruction titanium slag under high-temperature and high-pressure conditions, allows TiO then
2Substantially do not dissolve and make the stripping of impurity selectivity.
The used electro-titanium slag composition range of the present invention is:
TiO
2 80~87％，Al
2O
3 2~8％，SiO
2 2.5~4.5％，Fe 1~10％，
Mn 0.8~1.0％，MgO 1.3~1.8％，CaO＜0.5％
Granularity: 75%≤0.186mm.
The present invention realizes by implementing following technological process:
Its reparation technology comprises: High Temperature High Pressure leaches and liquid-solid separation circuit for the first time; In normal temperature and pressure leach and liquid-solid separation circuit for the second time; Washing and liquid-solid for the third time separation circuit; Rich titanium material drying process; The liquid waste disposal operation;
Described High Temperature High Pressure leach and for the first time liquid-solid separation circuit be: 120 ~ 145 ℃ of temperature, under pressure 0.2 ~ 0.4MPa condition, concentration is that the NaOH solution of 30 ~ 180g/l can be got the effect that destroys the titanium slag Solid solution, this procedure can stripping part Si O2, after realizing liquid-solid separation, the foreign matter content of titanium slag can reduce by 2 ~ 3%;
In described normal temperature and pressure leach and for the second time liquid-solid separation circuit be: 70 ~ 90 ℃ of temperature, the Solid solution structure is suffered that destructive titanium slag concentration is the H of 20 ~ 100g/l
2SO
4Solution leaches, and vitriolic consumption and other leaching condition are got the effect of selectivity stripping impurity and the few stripping of restricted T iO2, realize liquid-solid separation after, the TiO2 content of titanium slag reaches ~ 90%;
Described washing and liquid-solid for the third time separation circuit are: stir with hot water and wash out normal temperature and leach residual acid in the filter residue, realize liquid-solid separation after, the TiO2 of titanium slag 〉=90%, MgO+CaO＜2.0%;
Described rich titanium material drying process is: washing back titanium slag contains moisture ~ 11%, uses the high-temp waste gas drying to fall the free-water of titanium slag, and dry the end obtains the titanium slag of TiO2 〉=90%, MgO+CaO＜2.0%, moisture content≤2%;
Described liquid waste disposal is: High Temperature High Pressure is leached and for the first time the filtrate cycle in the liquid-solid separation circuit use, reduce the consumption of NaOH, as filtrate SiO
2When concentration reaches 22-26g/l, from flow process, open a way, as liquid waste disposal; Middle temperature leaches the disposable discharge of filtrate, handles with common process as waste liquid.
The reagent that adds is NaOH or H
2SO
4The concentration of reagent N aOH solution is 35 ~ 180g/l; Reagent H
2SO
4The concentration of solution is 20 ~ 100g/l.
Preferably 120 ~ 140 ℃ of the temperature that High Temperature High Pressure leaches; Pressure is 0.2 ~ 0.4MPa preferably.
In normal temperature and pressure leach and for the second time the temperature in the liquid-solid separation circuit preferably be controlled at about 80 ℃.
Work as filtrate SiO in the liquid waste disposal process
2When concentration reached 23-24g/l, filtrate must be opened a way from flow process, as liquid waste disposal.
The composition of the rich titanium material of producing is: TiO
2〉=90%, MgO+CaO＜2.0%.
The present invention utilizes TiO
280 ~ 87% titanium slags are produced TiO
2The processing method of 〉=90% rich titanium material, it has that flow process is short, energy consumption and low, the low cost and other advantages of water consumption, and refuse and wastewater flow rate that technological process produced are few, mineral compound such as mainly only siliceous in the waste water, aluminium, iron, magnesium, manganese, but handle just qualified discharge a little, little to environmental influence.The simple valid genus of process for treating waste liquor, the processed waste water allow compliance with emission standards, the secondary residue of handling the waste water generation meets the stacking standard.
Description of drawings: Fig. 1 is the process flow diagram of a kind of processing method with the rich titanium material of electro-titanium slag system of invention.
The major equipment of realizing the technical process of this invention is: autoclave and attached auxiliary facility, solid-liquid separating equipment, mechanical agitating tank, subsider, the pump of all size, storage tank, dry kiln etc.
Embodiment: production process of the present invention describes in detail:
High Temperature High Pressure leaches and liquid-solid separation for the first time, NaOH solution and electro-titanium slag after mixing, pulp groove 1 are continuously pumped in the autoclave, autoclave steam jacket heat supply, in establish agitator and stir 2h, material leaches under high-temperature and high-pressure conditions, discharges continuously from autoclave through leaching the back, is continuously pumped into semi-automatic squeezing machine with pump and carries out the solid-liquid separation first time, the filtrate that obtains is returned the recirculation of titanium slag tempering tank and is used, and filter residue is discharged into pulp groove 1.
Middle temperature leaches and liquid-solid separation for the second time, with H
2SO
4Solution and High Temperature High Pressure leach filter residue and pump in the mechanical agitating tank 1 after pulp groove 2 mixes, mechanical agitating tank steam direct heating, under normal pressure and comparatively high temps stirring, leach, after the leaching, pump into semi-automatic squeezing machine with pump and carry out the solid-liquid separation second time, the filtrate pumping wastewater treatment that obtains, filter residue is discharged into pulp groove 3.
Washing and liquid-solid for the third time separating technology, normal temperature leaches filter residue and hot water pumps into washing in the mechanical agitating tank 2 after pulp groove 3 mixes, washing finishes, pump into semi-automatic squeezing machine with pump and carry out solid-liquid separation for the third time, filtration back wash water returns the normal temperature leaching and is used for reagent preparation 2 solution, and filter residue focuses on.
Rich titanium material drying process, dry kiln is a thermal source with the high-temp waste gas of chlorination process technological process, high-temp waste gas enters with wet slag from kiln hood and makes inverse motion, emptying after gathering dust from kiln tail process then.The washing and filter pressing slag is continuously imported dry kiln with spiral from the kiln tail with the opening for feed of mechanical handling to dry kiln, discharges dry slag continuously from kiln hood, and all technology leaves it at that.
Process for treating waste liquor, waste liquid and the normal temperature leaching filtrate unification of High Temperature High Pressure after repeatedly circulating pumped into the liquid waste disposal pond, under agitation add reagent and control waste water terminal point PH=7 ~ 8, enter settling pool afterwards, qualified heavy clear water effluxes, and dense mud filters the back puts disposal as harmless slag muck.
Embodiment 1:
The some amounts of titanium slag, its composition are TiO
286.37%, Al
2O
36.35%, SiO
24.54%, Fe 2.36%, and Mn 0.79%, and MgO 1.32%, CaO＜0.05%; The first step is in 3 times of solution amount input autoclaves with titanium slag and NaOH concentration 120g/l, at pressure 0.4MPa temperature ~ 145 ℃ of following stirring reaction 2h; In second step, alkali soaked filter residue and sulfuric acid concentration is in 3 times of solution amount input mechanical agitating tanks of 50g/l, in 90 ℃ of following stirring reaction 2h; In the 3rd step, acidleach is crossed filter residue with 3 times of hot water amount's agitator treating 0.5h; In the 4th step, wash the after-filtration slag and send into the dry kiln drying, the check of dried feed timing sampling, warehouse-in at last.
The rich titanium material of gained content composition is TiO
291.15%, Al
2O
34.98%, SiO
22.05%, Fe 1.17%, and Mn 0.33%, and MgO 1.15%, CaO＜0.05%.
Embodiment 2 ~ 4
Get three parts of identical titanium slags, its composition is TiO
286.37%, Al
2O
36.35%, SiO
24.54%, Fe 2.36%, and Mn 0.79%, and MgO 1.32%, CaO＜0.05%; The first step is 30g/l with titanium slag and NaOH concentration, 80g/l, and 2 times of solution amount of 180g/l drop in the autoclave, at pressure 0.2MPa temperature ~ 120 ℃ of following stirring reaction 2h; In second step, alkali soaked filter residue and H
2SO
4Concentration is that 3 times of solution amount of 25g/l drop in the mechanical agitating tank, in 70 ℃ of following stirring reaction 2h; In the 3rd step, acidleach is crossed filter residue with 3 times of hot water amount's agitator treating 0.5h; In the 4th step, wash the after-filtration slag and send into the dry kiln drying, the check of dried feed timing sampling, warehouse-in at last.
The TiO of the rich titanium material of gained
2Content sees Table 1.
Rich titanium material TiO under the different basicity of table 1 uniform acidity
2Content
| Numbering | NaOH concentration (g/l) | H 2SO 4Concentration (g/l) | TiO 2Content (%) |
| Example 2 | 30 | 25 | 90.81 |
| Example 3 | 80 | 25 | 91.36 |
| Example 4 | 180 | 25 | 91.79 |
Embodiment 5 ~ 7
Get three parts of identical titanium slags, its composition is TiO
286.37%, Al
2O
36.35%, SiO
24.54%, Fe 2.36%, and Mn 0.79%, MgO1.32%, CaO＜0.05%; The first step is respectively titanium slag and NaOH concentration in 2 times of solution amount input autoclaves of 85g/l, at pressure 0.2MPa temperature ~ 120 ℃ of following stirring reaction 2h; In second step, alkali soaked filter residue respectively and H
2SO
4Concentration is 20g/l, 50g/l, and 3 times of solution amount of 100g/l drop in the mechanical agitating tank, in 80 ℃ of following stirring reaction 2h; In the 3rd step, acidleach is crossed filter residue with 3 times of hot water amount's agitator treating 0.5h; In the 4th step, wash the after-filtration slag and send into the dry kiln drying, the check of dried feed timing sampling, warehouse-in at last.
The TiO of the rich titanium material of gained
2Content sees Table 2.
Rich titanium material TiO under the identical basicity different acidity of table 2
2Content
| Numbering | NaOH concentration (g/l) | H 2SO 4Concentration (g/l) | TiO 2Content (%) |
| Example 5 | 85 | 20 | 91.04 |
| Example 6 | 85 | 50 | 91.27 |
| Example 7 | 85 | 100 | 90.25 |
Embodiment 8 ~ 10
Get three parts of identical titanium slags, its composition is TiO
286.37%, Al
2O
36.35%, SiO
24.54%, Fe 2.36%, and Mn 0.79%, MgO1.32%, CaO＜0.05%; The first step is in 2 times of solution amount input autoclaves of 100g/l with titanium slag and NaOH concentration, is respectively 0.2MPa at pressure, 0.3MPa, and 0.4MPa, temperature is respectively 120 ℃, and 130 ℃, stirring reaction 2h under 140 ℃ the condition; In second step, alkali soaked filter residue and H
2SO
4Concentration is that 3 times of solution amount of 25g/l drop in the mechanical agitating tank stirring reaction 2h under 70 ℃, 80 ℃, 90 ℃ temperature; In the 3rd step, acidleach is crossed filter residue with 3 times of hot water amount's agitator treating 0.5h; In the 4th step, wash the after-filtration slag and send into the dry kiln drying, the check of dried feed timing sampling, warehouse-in at last.
The TiO of the rich titanium material of gained
2Content sees Table 3.
Rich titanium material TiO under table 3 differing temps, the pressure
2Content
| Numbering | The first step temperature (℃) | Pressure (MPa) | TiO 2Content (%) | Second Buwen's degree (℃) |
| Example 8 | 120 | 0.2 | 92.92 | 70 |
| Example 9 | 130 | 0.3 | 91.85 | 80 |
| Example 10 | 140 | 0.4 | 91.29 | 90 |
The rich titanium material composition of explained hereafter of the present invention meets the require TiO of chloride process titanium dioxide production to raw material
2〉=90%, MgO+CaO＜2.0%.
Claims (7)
1 one kinds of processing methodes with the rich titanium material of electro-titanium slag system is characterized in that employed raw material is an electro-titanium slag, and its composition is:
TiO
2 80~87％，Al
2O
3 2~8％，SiO
2 2.5~4.5％，Fe 1~10％，
Mn 0.8 ~ 1.0%, and MgO 1.3 ~ 1.8%, CaO＜0.5%, and granularity: 75%≤0.186mm,
Its reparation technology comprises: High Temperature High Pressure leaches and liquid-solid separation circuit for the first time; In normal temperature and pressure leach and liquid-solid separation circuit for the second time; Washing and liquid-solid for the third time separation circuit; Rich titanium material drying process; The liquid waste disposal operation;
Described High Temperature High Pressure leach and for the first time liquid-solid separation circuit be: 120 ~ 145 ℃ of temperature, under pressure 0.2 ~ 0.4MPa condition, concentration is that the NaOH solution of 30 ~ 180g/l can be got the effect that destroys the titanium slag Solid solution, and this procedure can stripping part Si O
2, realize liquid-solid separation after, the foreign matter content of titanium slag can reduce by 2 ~ 3%;
In described normal temperature and pressure leach and for the second time liquid-solid separation circuit be: 70 ~ 90 ℃ of temperature, the Solid solution structure is suffered that destructive titanium slag concentration is the H of 20 ~ 100g/l
2SO
4Solution leaches, and vitriolic consumption and other leaching condition are got the effect of selectivity stripping impurity and the few stripping of restricted T iO2, realize liquid-solid separation after, the TiO of titanium slag
2Content reaches ~ and 90%;
Described washing and liquid-solid for the third time separation circuit are: stir with hot water and wash out normal temperature and leach residual acid in the filter residue, realize liquid-solid separation after, the TiO of titanium slag
2〉=90%, MgO+CaO＜2.0%;
Described rich titanium material drying process is: the rich titanium material in washing back contains moisture ~ 11%, uses the high-temp waste gas drying, reduces free-water, and dry the end obtains the product of TiO2 〉=90%, MgO+CaO＜2.0%, moisture content≤2%;
Described liquid waste disposal is: High Temperature High Pressure is leached and for the first time the filtrate cycle in the liquid-solid separation circuit use, reduce the consumption of NaOH, as filtrate SiO
2When concentration reaches 22-26g/l, from flow process, open a way, as liquid waste disposal; Middle temperature leaches the disposable discharge of filtrate, handles with common process as waste liquid.
2, a kind of processing method with the rich titanium material of electro-titanium slag system according to claim 1 is characterized in that the reagent that adds is NaOH, H
2SO
4
3, a kind of processing method according to claim 1 and 2 with the rich titanium material of electro-titanium slag system, the concentration that it is characterized in that reagent N aOH solution is 35 ~ 180g/l; Reagent H
2SO
4The concentration of solution is 20 ~ 100g/l.
4, a kind of processing method with the rich titanium material of electro-titanium slag system according to claim 1 is characterized in that preferably 120 ~ 140 ℃ of the temperature that High Temperature High Pressure leaches; Pressure is 0.2 ~ 0.4MPa preferably.
5, a kind of processing method with the rich titanium material of electro-titanium slag system according to claim 1 is characterized in that in the liquid waste disposal process as filtrate SiO
2When concentration reached 23g/l, filtrate must be opened a way from flow process, as liquid waste disposal.
6, a kind of processing method according to claim 1 with the rich titanium material of electro-titanium slag system, in it is characterized in that normal temperature and pressure leach and for the second time the temperature in the liquid-solid separation circuit be preferably 80 ℃.
7, a kind of processing method with the rich titanium material of electro-titanium slag system according to claim 1 and 2 is characterized in that the composition of the rich titanium material produced is: TiO
2〉=90%, MgO+CaO＜2.0%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768673A (en) * | 2010-03-08 | 2010-07-07 | 中南大学 | Method for preparing titanium-rich material from titanium-containing slag |
| CN102139918A (en) * | 2011-02-18 | 2011-08-03 | 昆明冶金研究院 | Method for preparing high-grade synthetic rutile |
| CN103834812A (en) * | 2012-11-26 | 2014-06-04 | 贵阳铝镁设计研究院有限公司 | Method for preparing titanium-rich material from low-grade TiO2 slag |
| CN104178647A (en) * | 2014-09-02 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining grade of titanium slag smelted from titanium concentrate and method for smelting titanium slag from titanium concentrate |
| 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 |
| CN112520786A (en) * | 2020-12-01 | 2021-03-19 | 成都工业学院 | Acid-soluble titanium-rich material and preparation method and application thereof |
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| CN104803415B (en) | 2015-05-15 | 2016-06-15 | 云南民族大学 | A kind of method being prepared rutile by acid-dissolved titanium slag |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085737C (en) * | 1999-08-10 | 2002-05-29 | 中南工业大学 | Process for preparing Ti-enriched material from ilmenite concentrate |
| RU2215053C1 (en) * | 2002-03-22 | 2003-10-27 | Государственное учреждение Институт металлургии Уральского отделения РАН | Titanium-containing slag processing method |
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2005
- 2005-12-27 CN CNB2005100487545A patent/CN100455683C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768673A (en) * | 2010-03-08 | 2010-07-07 | 中南大学 | Method for preparing titanium-rich material from titanium-containing slag |
| CN102139918A (en) * | 2011-02-18 | 2011-08-03 | 昆明冶金研究院 | Method for preparing high-grade synthetic rutile |
| CN103834812A (en) * | 2012-11-26 | 2014-06-04 | 贵阳铝镁设计研究院有限公司 | Method for preparing titanium-rich material from low-grade TiO2 slag |
| CN104178647A (en) * | 2014-09-02 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining grade of titanium slag smelted from titanium concentrate and method for smelting titanium slag from titanium concentrate |
| CN104178647B (en) * | 2014-09-02 | 2016-06-08 | 攀钢集团攀枝花钢铁研究院有限公司 | The defining method of ilmenite concentrate smelting titanium slag grade and ilmenite concentrate smelting titanium slag method |
| 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 |
| CN112520786A (en) * | 2020-12-01 | 2021-03-19 | 成都工业学院 | Acid-soluble titanium-rich material and preparation method and application thereof |
| CN112520786B (en) * | 2020-12-01 | 2022-08-23 | 成都工业学院 | Acid-soluble titanium-rich material and preparation method and application thereof |
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