CN107935033B - A kind of technique that titanium-containing blast furnace slag prepares titanium white raw material - Google Patents
A kind of technique that titanium-containing blast furnace slag prepares titanium white raw material Download PDFInfo
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Abstract
The present invention relates to the techniques that a kind of titanium-containing blast furnace slag prepares titanium white raw material, comprising: step 1 prepares carbonaceous composite pellet containing using titanium-containing blast furnace slag, carbonaceous reducing agent and sodium agent as raw material；Carbonaceous composite pellet containing is carried out sodium processing by step 2, obtains sodium slag；Step 3 hydrolyzes after sodium slag is carried out crushing grinding, obtains hydrolysis residue and the first filtrate；Step 4 carries out acidleach to hydrolysis residue using diluted acid, obtains titaniferous liquid and first and crosses filter residue；The first filtrate is handled using white lime to obtain the second filtrate；Step 5 carries out boiling hydrolysis to titaniferous liquid, obtains spent acid and second and crosses filter residue, crosses filter residue to second and calcine, obtain titanium white raw material.The present invention uses the hot sodium process titanium-containing blast furnace slag of carbon, perovskite is changed into sodium titanate, it is changed into the unsetting metatitanic acid and recyclable sodium salt for dissolving in diluted acid after hydrolysis process, efficiently use titanium white enterprise spent acid, spent acid containing titanium hydrolysis is Ke Xunhuanliyong, and does not generate spent acid discharge.
Description
Technical field
The present invention relates to metallurgical solid waste technical field of comprehensive utilization more particularly to a kind of titanium-containing blast furnace slag to prepare titanium white raw material
Technique.
Background technique
Chinese 90% or more titanium resource is distributed in Panxi Diqu, mainly exists in the form of vanadium titano-magnetite, reserves
Reach 1,000,000,000 tons or more.Vanadium titano-magnetite is a kind of grandidierite of a variety of valuable element symbiosis such as iron, vanadium, titanium, after ore dressing about
50% titanium, 70% iron and vanadium enter iron ore concentrate, mainly recycle vanadium-bearing hot metal through blast furnace process later, titanium-containing blast furnace slag due to
Titanium grade is lower (about 20%), limits the economy of titanium recycling, and titanium-containing blast furnace slag is not utilized effectively, and takes heap
Processing is deposited, causes a large amount of losses of titanium resource, while soil is occupied and got worse with environmental problem.According to statistics, it is high to climb steel titaniferous
Clinker volume of cargo in storage is close to 70,000,000 tons, and every annual increment is about 3,000,000 tons, and ownership and yield are all very huge.
When handling titanium-containing blast furnace slag using traditional sulfuric acid process, there is a problem of that acid consumption is big, spent acid discharge amount is big, economically
It is uneconomical, environmental protection pressure is big.
Summary of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of titanium-containing blast furnace slag prepares the technique of titanium white raw material, to solve
The problem of certainly existing acid consumes big, spent acid discharge amount greatly and impacts to environment when existing sulfuric acid process processing titanium-containing blast furnace slag.
The purpose of the present invention is mainly achieved through the following technical solutions:
A kind of technique that titanium-containing blast furnace slag prepares titanium white raw material, comprising the following steps:
Step 1 prepares carbonaceous composite pellet containing using titanium-containing blast furnace slag, carbonaceous reducing agent and sodium agent as raw material；
Carbonaceous composite pellet containing is carried out sodium processing by step 2, obtains sodium slag；
Step 3 hydrolyzes after sodium slag is crushed, is ground, and obtains hydrolysis residue and the first filtrate；
Step 4 carries out acidolysis to hydrolysis residue using diluted acid, obtains titaniferous liquid and first and crosses filter residue；Using white lime to
One filtrate obtains the second filtrate after being handled；
Step 5 carries out boiling hydrolysis to titaniferous liquid, obtains spent acid and second and crosses filter residue, crosses filter residue to second and calcine,
Obtain titanium white raw material.
The present invention has the beneficial effect that: the present invention prepares titanium white raw material, sodium agent and carbonaceous reduction by titanium-containing blast furnace slag
Agent is added simultaneously, can significantly improve the sodium rate of titanium；Sodium agent cycles through sodium bicarbonate saturation precipitation and obtains, and substantially reduces
The cycle cost of sodium agent；Hydrolysis residue can directly obtain titanium white raw material through acidleach, hydrolysis two-step method processing, not by material composition
Limitation.
On the basis of above scheme, the present invention has also done following improvement:
Further, in the step 1, the molar ratio of acidic oxide is 1 in the sodium agent and the titanium-containing blast furnace slag
~1.5, acidic oxide is the mixture of titanium oxide, silica and aluminium oxide in the titanium-containing blast furnace slag.
Beneficial effect using above-mentioned further scheme is: the present invention selects above-mentioned molar ratio that can guarantee acidic oxide
Maximization is converted into corresponding sodium salt, and silicon, aluminium soluble impurity are removed in hydrolytic process, meanwhile, titanium hydrolyzes to form metatitanic acid, is the later period
Diluted acid dissolution prepare titanium white raw material provide basis.
Further, in the step 1, the molar ratio of the carbonaceous reducing agent and sodium agent is 1~1.2.
Beneficial effect using above-mentioned further scheme is: the sodium process of traditional titanium is converted the hot sodium of carbon by the present invention
Process improves the sodium rate of titanium.
Further, the carbonaceous reducing agent is at least one of coal dust, coke powder or graphite powder；The sodium agent is
Na2CO3Or NaHCO3At least one of.
The reason of above-mentioned carbonaceous reducing agent of present invention selection and sodium agent, is: the hydrolysate of Sodium Titanate in hydrolytic process
Metatitanic acid and NaOH, the solubility of NaOH in water is very big, the form of evaporative crystallization can only be taken to recycle, energy consumption compared with
Height, and NaHCO31/10 of solubility in water not as good as NaOH is precipitated directly to utilize or dry by saturated crystallization and be decomposed
To Na2CO3It utilizes, greatly reduces the cycle cost of sodium agent.
Further, in the step 2, the sodium processing is by the carbonaceous composite pellet containing at 1100 DEG C~1300 DEG C
Lower heat preservation 60min~120min.
The selection of temperature and time of the present invention is while to avoid temperature mistake in order to which the sodium process for guaranteeing titanium, silicon, aluminium is abundant
Height brings energy consumption and operational difficulty.
Further, in the step 3, the sodium slag is obtained after carrying out crushing grinding less than 80 mesh powders；By institute
It is (5~10) by liquid-solid ratio that powder, which is stated, in the deionized water lower than 50 DEG C: 1 hydrolysis 3~5 times, every time 20~40min.
The present invention improves surface area by grinding sodium slag, and improving hydrolysis efficiency can be true under selected hydrolysising condition
It protects sodium slag and hydrolyzes the metatitanic acid for obtaining being suitble to diluted acid dissolution completely under lower quantity of circulating water.
Preferably, the powder is pressed to liquid-solid ratio in the deionized water lower than 50 DEG C is (5.7~9.1): 1 hydrolysis 3~5
It is secondary, 20~40min every time.
Further, in the step 4, the diluted acid refers to that volume fraction is 10%~22% dilute hydrochloric acid or dilute sulphur
Acid.
The present invention selects the diluted acid of above-mentioned volume fraction to can satisfy the leaching requirement of metatitanic acid, and contains with titanium white enterprise spent acid
Amount is consistent, waste acid reuse can be reduced production cost.
Further, in the step 4, the hydrolysis residue is (15~20) by liquid-solid ratio with the diluted acid: after 1 mixes,
60min~120min is leached within the temperature range of being lower than 50 DEG C.
The above-mentioned liquid-solid ratio of the present invention, temperature range and time are lauched titanium in solution slag and leach completely, avoid shifting to an earlier date for titaniferous liquid
Acidolysis.
Further, in the step 4, NaHCO is obtained after carrying out carbon point reaction to second filtrate3Saturated solution and
NaHCO3Solid precipitating, the NaHCO3Saturated solution hydrolysis stage after the sodium slag carries out crushing grinding recycles, institute
State NaHCO3Solid precipitating is recycled as sodium agent.
Further, in the step 5, the titaniferous liquid is heated to 60min~120min under fluidized state and carries out water
Solution；Filter residue is crossed after pickling, washing in 800 DEG C~1000 DEG C calcining 60min~120min by described second, obtains titanium white original
Material.
The present invention carries out acidolysis and calcining respectively within the time of selection and temperature range, is in order to ensure titaniferous liquid acidolysis
Completely, it is completely converted into Titanium Dioxide Rutile Top grade after calcining, can be used as titanium white and prepare raw material.
The invention has the benefit that
(1) present invention uses the hot sodium process titanium-containing blast furnace slag of carbon, perovskite is changed into sodium titanate, at hydrolysis
It is changed into the unsetting metatitanic acid and recyclable sodium salt for dissolving in diluted acid after reason, since the concentration of acid is wanted in metatitanic acid dissolution
It asks very low, can use titanium white enterprise spent acid, spent acid containing titanium hydrolysis is Ke Xunhuanliyong, does not generate spent acid discharge；
(2) present invention produces the titanium white raw material that can directly utilize using titanium-containing blast furnace slag, and has reached sour, alkali pair and followed
Ring has greater advantage from environmental protection and economic benefit.
It in the present invention, can also be combined with each other between above-mentioned each technical solution, to realize more preferred assembled schemes.This
Other feature and advantage of invention will illustrate in the following description, also, certain advantages can become from specification it is aobvious and
It is clear to, or understand through the implementation of the invention.The objectives and other advantages of the invention can be by written specification, right
Specifically noted structure is achieved and obtained in claim and attached drawing.
Detailed description of the invention
Attached drawing is only used for showing the purpose of specific embodiment, and is not to be construed as limiting the invention, in entire attached drawing
In, identical reference symbol indicates identical component.
Fig. 1 is that titanium-containing blast furnace slag of the present invention prepares titanium white raw material process flow chart.
Specific embodiment
Specifically describing the preferred embodiment of the present invention with reference to the accompanying drawing, wherein attached drawing constitutes the application a part, and
Together with embodiments of the present invention for illustrating the principle of the present invention, it is not intended to limit the scope of the present invention.
A specific embodiment of the invention discloses the technique that a kind of titanium-containing blast furnace slag prepares titanium white raw material, by titaniferous
Blast furnace slag and carbonaceous reducing agent, sodium agent are mixed with carbonaceous pelletizing, the acidic oxides such as titanium, silicon, aluminium and sodium in heating process
Agent reacts to form the compounds such as sodium titanate, sodium metasilicate, sodium aluminate, and in hydrolytic process, sodium titanate hydrolyzes to form metatitanic acid and hydrogen
Sodium oxide molybdena enters aqueous solution together with the soluble salts such as the latter and sodium metasilicate, sodium aluminate, filtering is realized be separated by solid-liquid separation after, filtered fluid warp
Recycling sodium agent recycles after lime removal of impurities, crosses filter residue through diluted acid leaching, hydrolysis, filtration treatment and obtains titanium white raw material, spent acid
It recycles, comprising the following steps:
A) with titanium-containing blast furnace slag, sodium agent (Na2CO3Or NaHCO3), carbonaceous reducing agent (coal dust, coke powder, graphite powder) be original
Material prepares carbonaceous pelletizing, wherein mole of sodium agent and acidic oxide (titanium oxide, silica, aluminium oxide) in titanium-containing blast furnace slag
Than being 1~1.5；Titanium, aluminium, silicon occur in 1100 DEG C~1300 DEG C heat preservation 60min~120min, heating process for carbonaceous pelletizing
Sodium process, titanium mainly exists in the form of Sodium Titanate after the reaction was completed；Said ratio is different from previous titanium-containing blast furnace slag
Alkaline process treatment process, the present invention relates to a kind of completely new hot sodium processes of carbon, as shown in formula (1)；The addition of carbonaceous reducing agent is aobvious
The sodium efficiency for improving titanium is write,
CaTiO3+Na2CO3+ C=Na2TiO3+CaO+2CO(g) (1)
B) above-mentioned sodium slag presses liquid-solid ratio (5 through crushing grinding to < 80 mesh powders in the deionized water lower than 50 DEG C
~10): filtering, which is realized, after 1 hydrolysis 30min is separated by solid-liquid separation, and filtered fluid is obtained after such 3 times and crosses filter residue, at this point, sodium titanate is sent out
Raw hydrolysis forms metatitanic acid precipitating and sodium hydroxide, sodium hydroxide enter filtered fluid together with sodium metasilicate, sodium aluminate；
Na2TiO3+3H2O=2NaOH+H4TiO4 (2)
Filtered fluid is after white lime removes silicon, aluminium impurity, then converts sodium bicarbonate for sodium hydroxide through carbon point reaction and satisfy
And precipitation, the evaporating concentration process of solution is avoided, the circulating consumption of sodium agent is substantially reduced；
Na2SiO3+Ca(OH)2=2NaOH+CaSiO3 (3)
2NaAlO2+Ca(OH)2=2NaOH+CaAl2O4 (4)
NaOH+CO2=NaHCO3 (5)
C) titanium mainly exists in the form of unbodied metatitanic acid in above-mentioned hydrolysis residue, also contains a small amount of perovskite, the former is low
Diluted acid is easily soluble under temperature, and perovskite is relatively insoluble in diluted acid.The dilute hydrochloric acid for being 10%~22% by hydrolysis residue and volume fraction
Or dilute sulfuric acid presses liquid-solid ratio (15~20): after 1 mixing, 60min~120min, filtering are leached within the temperature range of being lower than 50 DEG C
Obtain titaniferous liquid and solid residue, wherein the dissolution rate of titanium is 78%~93%；
H4TiO4+ 4HCl=TiCl4+4H2O (6)
H4TiO4+2H2SO4=Ti (SO4)2+4H2O (7)
D) above-mentioned titaniferous liquid heats 60min~120min under fluidized state and is hydrolyzed, and titanium chloride or titanium sulfate are in height
The lower hydrolysis of temperature re-forms metatitanic acid, and titanium-contained slag and hydrolysis acid solution are obtained by filtration after cooling, recycles after acid solution is concentrated, mistake
Filter residue, in 800 DEG C~1000 DEG C calcining 60min, obtains the richness of grade of titanium dioxide 96%~98% after pickling, washing process
Titanium material, can be directly as preparing titanium white raw material；
TiCl4+4H2O=H4TiO4+4HCl (8)
Ti(SO4)2+4H2O=H4TiO4+2H2SO4 (9)
Another specific embodiment of the invention discloses the technique that a kind of titanium-containing blast furnace slag prepares titanium white raw material, titaniferous
Blast furnace slag passes through the hot natridization reaction of carbon, and acidic oxide silicon, aluminium, titanium are separately converted to sodium metasilicate, sodium aluminate and sodium titanate in slag,
Hydrolysis properties based on sodium titanate, sodium ion are segregated into solution with titanium in hydrolytic process and recycle, will not be to titanium slag grade
It impacts, meanwhile, part Al, Si soluble salt enters aqueous solution, and the initial gross separation of titanium and impurity may be implemented；Titanium in hydrolysis residue
Transformation occurs again and forms metatitanic acid for sour sodium, and the latter is soluble in dilute hydrochloric acid or dilute sulfuric acid, realizes the two of titanium and impurity after separation of solid and liquid
Secondary separation；Titaniferous liquid obtains metatitanic acid through boiling hydrolysis again, and filtering realization titanium separates three times with impurity, and purity finally can be obtained
Up to 96~98% titanium slag is directly as titanium white raw material, and requirement of the acidleach process to acid concentration is lower, the recyclable benefit of spent acid
With.
Another specific embodiment of the invention discloses the technique that a kind of titanium-containing blast furnace slag prepares titanium white raw material, specifically
It is as follows:
Embodiment 1
In high-titanium blast furnace slag used in the present embodiment: TiO2Content 20.86%, CaO content 25.62%, SiO2Content
24.41%, Al2O3Content 12.65%, MgO 9.88%.By above-mentioned high-titanium blast furnace slag, Na2CO3It is mixed in proportion with graphite powder
It closes and uniformly prepares carbonaceous composite pellet containing, wherein Na2CO3As sodium agent, graphite powder is as carbonaceous reducing agent, carbonaceous composite pellet containing
Middle Na2CO3Additional amount and titanium-containing blast furnace slag acidic oxide molar ratio be 1.5, the additional amount and Na of graphite powder2CO3Mass ratio
It is 0.115；Acidic oxide refers to the total amount of titanium oxide, silica and aluminium oxide.
The hot sodium of carbon is carried out in 1150 DEG C~1300 DEG C corundum crucible inside holding 120min after carbonaceous composite pellet containing is dried
Processing takes out cooling after reaching soaking time, obtains sodium slag.Sodium slag is prepared into < 80 purposes on swing crushing sampling machine
Powdered sample is filtered after persistently stirring hydrolyzes 30min in lower than 50 DEG C, the deionized water that liquid-solid ratio is 10:1, is filtered
Liquid and hydrolysis residue, the NaOH generated containing sodium titanate hydrolysis in filtered fluid and the sodium metasilicate and sodium aluminate that are dissolved in water, through lime
Recycling sodium agent recycles after removing silicon, aluminium impurity；
Hydrolysis residue prepares titanium white raw material through acid system leaching process, hydrolysis residue liquid-solid ratio be 15:1, concentration be 10% it is dilute
Salt Ore Leaching 120min obtains titaniferous liquid and the solid residue insoluble in diluted acid after separation of solid and liquid；
It is noted that dissolution rate of the titanium in 10% dilute hydrochloric acid is 78% when the hot sodium temperature of carbon is 1150 DEG C, when
When temperature is increased to 1200 DEG C, the dissolution rate of titanium is improved to 83%, and the leaching rate of titanium is 81% when temperature is 1300 DEG C.
Case 2
The ingredient of high-titanium blast furnace slag in the present embodiment and the preparation method of carbonaceous composite pellet containing are same as Example 1.
Titaniferous liquid obtained in embodiment 1 is heated to boiling and 120min is kept to be hydrolyzed, is analysed again under high temperature
Metatitanic acid precipitates out, is separated by solid-liquid separation again after cooling by vacuum apparatus, crosses filter residue through 5% dilute hydrochloric acid pickling, deionized water 3
It is dried after secondary washing, titanium grade reaches 96~98% in 950 DEG C of calcining 60min, obtained high titanium slag, can be directly as system
The raw material of standby titanium white.
The hydrolysis residue that 1200 DEG C of sodiums processing slag is obtained through crushing grinding, hydrolysis process, liquid-solid ratio is 15:1, concentration is
After 10% dilute hydrochloric acid leaches 120min, solidliquid mixture is directly heated to boiling hydrolysis, what is obtained after filtering crosses filter residue warp
It is dried after 5% dilute hydrochloric acid pickling, deionized water 3 times washings, titanium grade is in 950 DEG C of calcining 60min, obtained high titanium slag
93.4%.
This shows that the titanium slag quality obtained using two-step process is higher than one-step technology.
Embodiment 3
The ingredient of high-titanium blast furnace slag in the present embodiment and the preparation method of carbonaceous composite pellet containing are same as Example 1.
The hydrolysis residue that 1200 DEG C of sodium processing slags are obtained through crushing grinding, hydrolysis-washing process, presses liquid with 22% dilute sulfuric acid
Gu being realized and being separated by solid-liquid separation by vacuum apparatus after 15:1 mixing acidleach 120min, 93% titanium dissolution enters liquid phase.This
Show that dilute sulfuric acid is stronger than dilute hydrochloric acid to the solvability of titanium in hydrolysis residue.
Titaniferous liquid is boiled and hydrolyzes 120min, is separated by solid-liquid separation after cooling, filter residue is through 5% dilute sulfuric acid pickling, deionized water 3 times
It is dried after washing, after 950 DEG C of calcining 60min, titanium grade reaches 97.3% in slag.
In conclusion the present invention provides the technique that a kind of titanium-containing blast furnace slag prepares titanium white raw material, using the hot sodium work of carbon
Skill handles titanium-containing blast furnace slag, and perovskite is changed into sodium titanate, is changed into the unsetting titanium for dissolving in diluted acid after hydrolysis process
Acid and Ke Xunhuanliyong sodium salt can use titanium white enterprise spent acid, contain since concentration requirement of the metatitanic acid dissolution to acid is very low
Titanium hydrolysis spent acid is Ke Xunhuanliyong, does not generate spent acid discharge.Therefore, the present invention can be utilized directly using titanium-containing blast furnace slag production
Titanium white raw material, and reached acid, alkali Two-way Cycle, from environmental protection and economic benefit have greater advantage.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (6)
1. the technique that a kind of titanium-containing blast furnace slag prepares titanium white raw material, which is characterized in that the technique specifically:
Step 1 prepares carbonaceous composite pellet containing using titanium-containing blast furnace slag, carbonaceous reducing agent and sodium agent as raw material；
Carbonaceous composite pellet containing is carried out sodium processing by step 2, obtains sodium slag；
Step 3 hydrolyzes after sodium slag is crushed, is ground, and obtains hydrolysis residue and the first filtrate；
Step 4 carries out acidleach to hydrolysis residue using diluted acid, obtains titaniferous liquid and first and crosses filter residue；It is filtered using white lime to first
Liquid obtains the second filtrate after being handled；
Step 5 carries out boiling hydrolysis to titaniferous liquid, obtains spent acid and second and crosses filter residue, crosses filter residue to second and calcine, obtain
Titanium white raw material；
In the step 3, the sodium slag is obtained after carrying out crushing grinding less than 80 mesh powders；The powder is being lower than 50
DEG C deionized water in by liquid-solid ratio be (5~10): 1 hydrolysis 3~5 times, every time 20~40min；
In the step 4, the diluted acid refers to that volume fraction is 10%~22% dilute hydrochloric acid or dilute sulfuric acid；
In the step 4, the hydrolysis residue is (15~20) by liquid-solid ratio with the diluted acid: after 1 mixes, being lower than 50 DEG C of temperature
It spends and leaches 60min~120min in range；
In the step 5, the titaniferous liquid is heated to 60min~120min under fluidized state and is hydrolyzed；By described second
Filter residue is crossed after pickling, washing in 800 DEG C~1000 DEG C calcining 60min~120min, obtains titanium white raw material.
2. the technique that a kind of titanium-containing blast furnace slag according to claim 1 prepares titanium white raw material, which is characterized in that the step
In 1, the molar ratio of acidic oxide is 1~1.5 in the sodium agent and the titanium-containing blast furnace slag, acid in the titanium-containing blast furnace slag
Property oxide be titanium oxide, silica and aluminium oxide mixture；The molar ratio of the carbonaceous reducing agent and sodium agent is 1~
1.2。
3. the technique that a kind of titanium-containing blast furnace slag according to claim 1 prepares titanium white raw material, which is characterized in that the carbonaceous
Reducing agent is at least one of coal dust, coke powder or graphite powder；The sodium agent is Na2CO3Or NaHCO3At least one of.
4. the technique that a kind of titanium-containing blast furnace slag according to claim 1 prepares titanium white raw material, which is characterized in that the step
In 2, the sodium processing is that the carbonaceous composite pellet containing is kept the temperature to 60min~120min at 1100 DEG C~1300 DEG C.
5. the technique that a kind of titanium-containing blast furnace slag according to claim 1 prepares titanium white raw material, which is characterized in that by the powder
End is (5.7~9.1) by liquid-solid ratio in the deionized water lower than 50 DEG C: 1 hydrolysis 3~5 times, every time 20~40min.
6. the technique that a kind of titanium-containing blast furnace slag according to claim 3 prepares titanium white raw material, which is characterized in that the step
In 4, NaHCO is obtained after carrying out carbon point reaction to second filtrate3Saturated solution and NaHCO3Solid precipitating, the NaHCO3
Saturated solution hydrolysis stage after the sodium slag carries out crushing grinding recycles, the NaHCO3Solid precipitating is used as sodium
Agent recycles.
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