CN104944466B - A kind of wet method prepares the production method of rich-titanium material - Google Patents
A kind of wet method prepares the production method of rich-titanium material Download PDFInfo
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Abstract
The invention discloses a kind of wet method and prepare the production method of rich-titanium material, including the acquisition of acid titanium liquid, the acquisition of reduction titanium, preparation rich-titanium material, the processing step of this production method is: add in premix tank by the concentrated sulfuric acid or hydrochloric acid or sulfuric acid and the mixed liquor of hydrochloric acid and ilmenite, it is then added in acidolysis pot, add and cause liquid, obtain acid hydrolysate；Dilution obtains acid titanium liquid；By calcined by rotary kiln after ilmenite concentrate, fine coal being mixed, kiln discharge magnetic separation obtains reduction titanium；Acid titanium is filtrated to get the acid titanium liquid of high cleanliness；The titanium that step reduced adds in the acid titanium liquid of high cleanliness and reduces；When there is titanous in titanium liquid, reduction terminates；Separation of solid and liquid；Solid formation is dried to obtain rich-titanium material.This invention can produce a kind of rich-titanium material meeting chloridising needs, i.e. can save the consumption of electro-smelting mass energy, can be again that sulfate process titanium dioxide produces a kind of new development model of offer.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of with reduction titanium prepare rich-titanium material for raw material wet method
Production method.
Background technology
Titanium dioxide is optimal Chinese white, is widely used in coating, papermaking, plastics, rubber, chemical fibre, ink, doctor
The industrial circles such as, food.
The industrialized production of titanium dioxide started from for 20 beginnings of the century, and common method has sulfuric acid process, chloridising two kinds.China's titanium white
Powder industry is based on sulfuric acid process, and its primary raw material is ilmenite, ilmenite Titanium White Production By Sulfuric Acid Process, can the substantial amounts of sulphur of output
Acid ferrous iron and spent acid.By producing based on 1 ton of titanium white, by dense for output spent acid 7～8 tons, green vitriol 3～3.5 tons, acid waste water 150～250
Ton, causes serious destruction to environment.Therefore, along with improving constantly of people's environmental consciousness, chloride process titanium dioxide will go from strength to strength.
At present, the demand of chloride process titanium dioxide raw material is improved by market day by day, and chloridising produces titanium white to be had higher to raw material
Requirement, except improving in addition to grade of titanium dioxide, also require that MgO+CaO content sum can not be more than 1.5%.Chloride process titanium dioxide is former
Material mainly high titanium slag or synthetic rutile.
The most industrial application produces the method for rich-titanium material mainly three kinds: electric furnace smelting process, the acid-hatching of young eggs and reduction
Bubble method.The raw material used is mainly ilmenite.Electric furnace smelting process is simple and reliable, can obtain rich-titanium material and pig two kinds simultaneously
Product, but power consumption is big, is only limitted to the area use that electric power is sufficient, and fusion process is primarily discrete except iron, removes non-ferrous impurities energy
Power is poor.The acid-hatching of young eggs is big due to " three wastes " amount, and sidestream journey is complicated, thus limits its application.Reductive leaching is then only applicable to
Process high-grade ore in sand form.
Therefore, it is necessary to seek the new method producing rich-titanium material, work hard to complete the upgrading of rich-titanium material product refinement method.
Summary of the invention
It is an object of the invention to the defect for above-mentioned prior art, it is provided that a kind of wet method prepares the producer of rich-titanium material
Method, can refine low-grade ore in sand form, overcome the defect that electro-smelting mass energy consumes, and produces for sulfate process titanium dioxide
A kind of new quality kind benefit is provided to refine pattern.
To achieve these goals, the technical scheme is that
A kind of wet method prepares the production method of rich-titanium material, including the acquisition of acid titanium liquid, the acquisition of reduction titanium, the rich titanium of preparation
Material, the processing step of this production method is:
A. the acquisition of acid titanium liquid
A1. the concentrated sulfuric acid or hydrochloric acid are added in premix tank, be subsequently adding ilmenite, stirring；
A2. the mixed liquor that step A1 obtains is joined in acidolysis pot, add and cause liquid, make the mixed liquor that step A1 obtains
There is acidolysis reaction, obtain acid hydrolysate；
A3. acid hydrolysate step A2 obtained adds dilution so that sulfate or chlorate in acid hydrolysate are molten
Solve, obtain acid titanium liquid；
B. the acquisition of titanium is reduced
B1. joined in rotary kiln by rotary kiln after ilmenite concentrate, fine coal being mixed and calcine, carry out pre-oxidation and go back in advance
Former, obtain calcining materials；
B2. being transferred to the calcining materials obtained cool down in kiln cool down, kiln discharge magnetic separation obtains reduction titanium；
C. rich-titanium material is prepared
C1. the acid titanium liquid obtained by step A is added flocculant solution, after stirring impurity elimination, is filtrated to get the acid of high cleanliness
Property titanium liquid；
C2. the reduction titanium obtained by step B is added in the acid titanium liquid of the high cleanliness obtained by step C1 and carry out also
Former；When there is titanous in titanium liquid, reduction terminates；
C3. separation of solid and liquid；Obtain solid formation；
C4. solid formation is dried to obtain rich-titanium material.
As the improvement to technique scheme, in described step A1, the concentration of the described concentrated sulfuric acid is 92～94%, institute
Stating concentration of hydrochloric acid is 28-33%, and the sour ore deposit mass ratio of the described concentrated sulfuric acid or hydrochloric acid and ilmenite is 1.50～1.70；
As the improvement to technique scheme, in described step A2, described initiation liquid is the spent acid of water or 5-20%；
In described acidolysis reaction, from the start to finish of acidolysis reaction, the concentration of reaction acid solution controls 81～89%, described acid
The time solving reaction is 20～40min.
As the improvement to technique scheme, in described step A3, described dilution is the spent acid of water or 5-20%,
In obtained acid titanium liquid, the concentration of total titanium is 110～120g/L.
As the improvement to technique scheme, in described step B1, described ilmenite concentrate and the mass ratio adding fine coal
For 1:0.01～0.1；Spraying into coal dust at kiln hood coal powder lance, the coal dust sprayed into is 0.05 with the mass ratio of described ilmenite concentrate simultaneously
～0.4:1；Calcining heat is 1000～1200 DEG C, and calcination time is 3-24h；Calcining simultaneously, mends wind from kiln hood and kiln body.
As the improvement to technique scheme, in described step B2, cooling means is cold or air cooling of spraying water, after cooling
The temperature of material is 30～50 DEG C.
As the improvement to technique scheme, in described step B2, described magnetic separation uses many magnetic poles equipment to carry out multistage
Magnetic separation separates, and the magnetic field intensity of the many magnetic poles equipment carrying out multi-stage magnetic separation separation is 3000～10000GS.
As the improvement to technique scheme, in described step C1, the mass fraction of described flocculant solution is
1 ‰, acid titanium liquid is 13:91 with the volume ratio of flocculant solution.
As the improvement to technique scheme, in described step C2, during reduction, the temperature of titanium liquid controls 30～75
DEG C, the time of reduction reaction is 0.5～1h.
Compared with prior art, the invention has the beneficial effects as follows:
1. the inventive method belongs to liquid phase wet method and prepares rich-titanium material, compared with high melt method, can save substantial amounts of energy
Source consumes.Compared with the acid-hatching of young eggs, the discharge of " three wastes " can be stopped；
2. reduction titanium is used for reducing titanium liquid, consumes metallic iron therein, not only eliminates the consumption of iron powder, simultaneously titanium liquid
In it also avoid introducing other impurity elements, improve titanium dioxide quality, rich-titanium material of simultaneously having got back product；
3. the raw material that the byproduct ferrous sulfate obtained after reduction titanium liquid can produce as iron pigment, meets country and carries
The green circulation economy development model advocated.
4. after reduction titanium replaces iron powder reducing titanium liquid, ton titanium white can save iron powder about 140 kilograms: is worth 350 yuan, consumes
Reduction titanium about 420 kilograms, is worth 2100 yuan, produces high titanium slag about 280 kilograms simultaneously, is worth 2464 yuan, amounts to ton titanium white
Benefit 714 yuan can be obtained, based on producing 200000 tons per year, benefit more than 100,000,000 yuan can be obtained every year.
Low-grade ore in sand form can be refined by the present invention, overcomes the defect that electro-smelting mass energy consumes, for sulphur
Acid system Producing Titanium Dioxide provides a kind of new quality kind benefit to refine pattern.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
The wet method of the present embodiment prepares the processing step of the production method of rich-titanium material:
A. the acquisition of acid titanium liquid
A1. 92% concentrated sulfuric acid is added in premix tank, be subsequently adding ilmenite, stirring；The concentrated sulfuric acid and the sour ore deposit of ilmenite
Mass ratio is 1.50；
A2. joining in acidolysis pot by the mixed liquor that step A1 obtains, add water and make to cause liquid, make that step A1 obtains is mixed
Close liquid generation acidolysis reaction, obtain acid hydrolysate；From the start to finish of acidolysis reaction, the concentration of reaction acid solution controls 81%；
The time of described acidolysis reaction is 20min；
A3. acid hydrolysate step A2 obtained adds water and makees dilution so that the sulfate in acid hydrolysate dissolves,
To acid titanium liquid, in obtained acid titanium liquid, the concentration of total titanium is 110g/L.
B. the acquisition of titanium is reduced
B1. joined in rotary kiln by rotary kiln after ilmenite concentrate, fine coal being mixed for 1:0.01 in mass ratio and calcine,
Carry out pre-oxidizing and prereduction, spray into coal dust at kiln hood coal powder lance simultaneously, the coal dust sprayed into and the mass ratio of described ilmenite concentrate
For 0.05:1, calcining heat is 1000 DEG C, and calcination time is 3h；Calcining simultaneously, mends wind from kiln hood and kiln body, and calcining obtains after terminating
To calcining materials；
B2. being transferred to the calcining materials obtained cool down cold or air cooling of spraying water in kiln, being cooled to temperature is 30 DEG C, kiln discharge warp
Magnetic field intensity be 3000GS multi-stage magnetic separation equipment magnetic separation separate after obtain reduce titanium；
C. rich-titanium material is prepared
C1. the acid titanium liquid obtained by step A being added mass fraction is the flocculant solution of 1 ‰, acid titanium liquid and wadding
The volume ratio of solidifying agent solution is 13:91, is filtrated to get the acid titanium liquid of high cleanliness after stirring impurity elimination；
C2. the reduction titanium obtained by step B is added in the acid titanium liquid of the high cleanliness obtained by step C1 and carry out also
Former；When there is titanous in titanium liquid, reduction terminates；Reduction temperature controls at 30 DEG C, and the time of reduction reaction is 0.5h；
C3. separation of solid and liquid；Obtain solid formation；
C4. solid formation is dried to obtain rich-titanium material.
Embodiment 2
The wet method of the present embodiment prepares the processing step of the production method of rich-titanium material:
A. the acquisition of acid titanium liquid
A1. 28% hydrochloric acid is added in premix tank, be subsequently adding ilmenite, stirring；Hydrochloric acid and the sour mineral amount of ilmenite
Ratio is 1.70；
A2. joining in acidolysis pot by the mixed liquor that step A1 obtains, the spent acid adding 20% is made to cause liquid, makes step A1
The mixed liquor generation acidolysis reaction obtained, obtains acid hydrolysate；From the start to finish of acidolysis reaction, the concentration control of reaction acid solution
System is 86%；The time of described acidolysis reaction is 40min；
A3. acid hydrolysate step A2 obtained adds the spent acid of 5% and makees dilution so that the chlorate in acid hydrolysate
Dissolving, obtain acid titanium liquid, in obtained acid titanium liquid, the concentration of total titanium is 120g/L.
B. the acquisition of titanium is reduced
B1. joined in rotary kiln by rotary kiln after ilmenite concentrate, fine coal being mixed for 1:0.1 in mass ratio and calcine,
Carry out pre-oxidizing and prereduction, spray into coal dust at kiln hood coal powder lance simultaneously, the coal dust sprayed into and the mass ratio of described ilmenite concentrate
For 0.4:1, calcining heat is 1200 DEG C, and calcination time is 12h；Calcining simultaneously, mends wind from kiln hood and kiln body, and calcining obtains after terminating
To calcining materials；
B2. being transferred to the calcining materials obtained cool down cold or air cooling of spraying water in kiln, being cooled to temperature is 50 DEG C, kiln discharge warp
Magnetic field intensity be 10000GS multi-stage magnetic separation equipment magnetic separation separate after obtain reduce titanium；
C. rich-titanium material is prepared
C1. the acid titanium liquid obtained by step A being added mass fraction is the flocculant solution of 1 ‰, acid titanium liquid and wadding
The volume ratio of solidifying agent solution is 13:91, is filtrated to get the acid titanium liquid of high cleanliness after stirring impurity elimination；
C2. the reduction titanium obtained by step B is added in the acid titanium liquid of the high cleanliness obtained by step C1 and carry out also
Former；When there is titanous in titanium liquid, reduction terminates；Reduction temperature controls at 50 DEG C, and the time of reduction reaction is 0.75h；
C3. separation of solid and liquid；Obtain solid formation；
C4. solid formation is dried to obtain rich-titanium material.
Embodiment 3
A. the acquisition of acid titanium liquid
A1. 94% concentrated sulfuric acid is added in premix tank, be subsequently adding ilmenite, stirring；The concentrated sulfuric acid and the sour ore deposit of ilmenite
Mass ratio is 1.6；
A2. joining in acidolysis pot by the mixed liquor that step A1 obtains, add water and make to cause liquid, make that step A1 obtains is mixed
Close liquid generation acidolysis reaction, obtain acid hydrolysate；From the start to finish of acidolysis reaction, the concentration of reaction acid solution controls 89%；
The time of described acidolysis reaction is 30min；
A3. acid hydrolysate step A2 obtained adds the spent acid of 5% and makees dilution so that the sulfate in acid hydrolysate
Dissolving, obtain acid titanium liquid, in obtained acid titanium liquid, the concentration of total titanium is 115g/L.
B. the acquisition of titanium is reduced
B1. joined in rotary kiln by rotary kiln after ilmenite concentrate, fine coal being mixed for 1:0.05 in mass ratio and calcine,
Carry out pre-oxidizing and prereduction, spray into coal dust at kiln hood coal powder lance simultaneously, the coal dust sprayed into and the mass ratio of described ilmenite concentrate
For 0.1:1, calcining heat is 1100 DEG C, and calcination time is 24h；Calcining simultaneously, mends wind from kiln hood and kiln body, and calcining obtains after terminating
To calcining materials；
B2. being transferred to the calcining materials obtained cool down cold or air cooling of spraying water in kiln, being cooled to temperature is 40 DEG C, kiln discharge warp
Magnetic field intensity be 7000GS multi-stage magnetic separation equipment magnetic separation separate after obtain reduce titanium；
C. rich-titanium material is prepared
C1. the acid titanium liquid obtained by step A being added mass fraction is the flocculant solution of 1 ‰, acid titanium liquid and wadding
The volume ratio of solidifying agent solution is 13:91, is filtrated to get the acid titanium liquid of high cleanliness after stirring impurity elimination；
C2. the reduction titanium obtained by step B is added in the acid titanium liquid of the high cleanliness obtained by step C1 and carry out also
Former；When there is titanous in titanium liquid, reduction terminates；Reduction temperature controls below 75 DEG C, and the time of reduction reaction is 1h；
C3. separation of solid and liquid；Obtain solid formation；
C4. solid formation is dried to obtain rich-titanium material.
Compare with present certain titanium slag manufacturer situation with electro-smelting production rich-titanium material.
The GB of high titanium slag such as following table:
This titanium slag manufacturer gained rich-titanium material test case, analysis is analyzed with the produced x ray fluorescence spectrometry of PANalytical
As shown in the table by the method gained rich-titanium material situation of the present invention:
Knowable to data above contrasts, use the method for the present invention can obtain the rich-titanium material that content of calcium and magnesium is few, meet
The chloride process titanium dioxide requirement to raw material.
The granularity of comparative example and experiment case study sample is measured by state's calibration method.
As can be known from the table data, the rich-titanium material granularity using this method to prepare is concentrated mainly on～between 40 mesh+170 mesh,
Fine particles amount meets the requirement of GB.
It will be apparent from the above that, this invention can produce a kind of rich-titanium material meeting chloridising needs, i.e. can save electric furnace and melt
The consumption of refining mass energy, can be again that sulfate process titanium dioxide produces a kind of new development model of offer.
The above is only one embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement, these improvement also should be regarded as this
Bright protection domain.
Claims (8)
1. a wet method prepares the production method of rich-titanium material, it is characterised in that: include the acquisition of acid titanium liquid, the obtaining of reduction titanium
Obtaining, prepare rich-titanium material, the processing step of this production method is:
A. the acquisition of acid titanium liquid
A1. the concentrated sulfuric acid or hydrochloric acid are added in premix tank, be subsequently adding ilmenite, stirring；
A2. joining in acidolysis pot by the mixed liquor that step A1 obtains, add and cause liquid, the mixed liquor making step A1 obtain occurs
Acidolysis reaction, obtains acid hydrolysate；
A3. acid hydrolysate step A2 obtained adds dilution so that sulfate or chlorate in acid hydrolysate dissolve,
To acid titanium liquid；
B. the acquisition of titanium is reduced
B1. calcine being joined in rotary kiln by rotary kiln after ilmenite concentrate, fine coal mixing, carry out pre-oxidizing and prereduction,
Obtain calcining materials；
B2. being transferred to the calcining materials obtained cool down in kiln cool down, kiln discharge magnetic separation obtains reduction titanium；
C. rich-titanium material is prepared
C1. the acid titanium liquid obtained by step A is added flocculant solution, after stirring impurity elimination, is filtrated to get the acid titanium of high cleanliness
Liquid；
C2. the reduction titanium obtained by step B is added in the acid titanium liquid of the high cleanliness obtained by step C1 and reduce；When
When there is titanous in titanium liquid, reduction terminates；
C3. separation of solid and liquid；Obtain solid formation；
C4. solid formation is dried to obtain rich-titanium material.
Wet method the most according to claim 1 prepares the production method of rich-titanium material, it is characterised in that: in described step A1,
The concentration of the described concentrated sulfuric acid is 92～94%, and described concentration of hydrochloric acid is 28-33%, the described concentrated sulfuric acid or hydrochloric acid and the sour ore deposit of ilmenite
Mass ratio is 1.50～1.70.
Wet method the most according to claim 1 and 2 prepares the production method of rich-titanium material, it is characterised in that:
In described step A2, described initiation liquid is the spent acid of water or 5-20%；In described acidolysis reaction, from acidolysis reaction
Start to finish, reaction acid solution concentration control 81～89%, the time of described acidolysis reaction is 20～40min.
Wet method the most according to claim 3 prepares the production method of rich-titanium material, it is characterised in that: in described step A3,
Described dilution is the spent acid of water or 5-20%, and in obtained acid titanium liquid, the concentration of total titanium is 110～120g/L.
Wet method the most according to claim 1 prepares the production method of rich-titanium material, it is characterised in that: in described step B2,
Cooling means is cold or air cooling of spraying water, and after cooling, the temperature of material is 30～50 DEG C.
Wet method the most according to claim 5 prepares the production method of rich-titanium material, it is characterised in that: in described step B2, institute
Stating magnetic separation uses many magnetic poles equipment to carry out multi-stage magnetic separation separation, and the magnetic field intensity of the many magnetic poles equipment carrying out multi-stage magnetic separation separation is
3000～10000GS.
Wet method the most according to claim 1 prepares the production method of rich-titanium material, it is characterised in that: in described step C1,
The mass fraction of described flocculant solution is 1 ‰, and acid titanium liquid is 13:91 with the volume ratio of flocculant solution.
8. the production method of rich-titanium material is prepared according to the wet method described in claim 1 or 7, it is characterised in that: in described step C2
In, during reduction, the temperature of titanium liquid controls at 30～75 DEG C, and the time of reduction reaction is 0.5～1h.
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| CN108217723B (en) * | 2018-03-08 | 2020-03-20 | 四川龙蟒钛业股份有限公司 | Method for effectively improving acidolysis productivity |
| CN111471868B (en) * | 2020-05-14 | 2021-08-27 | 龙蟒佰利联集团股份有限公司 | Method for recycling flue gas dust of titanium slag electric furnace |
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