CN106115778A - The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag - Google Patents
The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag Download PDFInfo
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- CN106115778A CN106115778A CN201610494517.XA CN201610494517A CN106115778A CN 106115778 A CN106115778 A CN 106115778A CN 201610494517 A CN201610494517 A CN 201610494517A CN 106115778 A CN106115778 A CN 106115778A
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- acidolysis
- slag
- sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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Abstract
The present invention relates to a kind of sulfate process titanium dioxide powder craft, specifically disclose the recoverying and utilizing method of a kind of sulfuric acid method titanium pigment acidolysis slag.The steps include: A, by acidolysis slag by selected raising Ti content, obtain the selected slag of acidolysis；B, by selected for acidolysis slag add wet ball mill levigate；C, levigate acidolysis slag filter pressing is dried up；D, addition sulphuric acid pump into acidolysis pot together with acidolysis ilmenite concentrate premix material mix making beating with filter press cake after and carry out acidolysis.It is an advantage of the current invention that: 1) improve acidolysis slag acidolysis rate；2) avoid coarse granule breeze vicious cycle because of acidolysis effect difference in the selected slag of acidolysis, cause production efficiency to decline；3) abundant Resource recovery, reduces debris dump high-volume.
Description
Technical field
The present invention relates to a kind of sulfuric acid method titanium pigment production technology, the process of a kind of sulfuric acid method titanium pigment acidolysis slag
Method.
Background technology
The primary raw material of sulfuric acid method titanium pigment production technology is ilmenite concentrate, and its composition is iron titanate, effective ingredient titanium dioxide
Titanium contains general 45%～55%.Outsourcing ilmenite concentrate is after Raymond mill or ball mill are pulverized, by amount of calculation in acidolysis pot
Mix with concentrated sulphuric acid, add water dilution, utilize the heat of dilution of concentrated sulphuric acid to cause acidolysis reaction, generate loose porous solid formation
Matter, through overcuring, add water extraction, add the operation such as iron powder reducing after become acidolysis titanium liquid, titanium liquid be mainly composed of sulphuric acid oxygen
The aqueous solution of titanium, ferrous sulfate and dilute sulfuric acid, in addition with a small amount of non-acidolysis ilmenite concentrate, shale mineral, pyroxene, magnalium point crystalline substance
Stone, hornblend, chlorite, olivine, quartz, magnetic iron ore and pyrite etc., the composition of these solid formations is with the thing of ilmenite concentrate
Matter composition changes and changes.In order to prepare the cleaning titanyl sulfate solution meeting titanium white production technological requirement, it is necessary under connecing
The operation come removes these solid phase impurity by sedimentation.In sedimentation operation, in acidolysis titanium liquid, add cationic flocculant
Catching the colloidal substance formed in these responseless solid particles and acidolysis, the clear titanium liquid on Sedimentation tank top is sent to follow-up work
Section, the part that a large amount of solid phase impurity is contained in lower floor is sent to follow-up workshop section by Filter Press, filtrate, and filter cake is generally as discarded
Thing is stacked, owing to this filter cake is to be commonly referred to as acidolysis slag in acid hemolysis process in responseless material composition, industry.
This acidolysis slag typically contains the moisture of about 25%, the soluble titanium dioxide of about 3%, about 8%
Sulphuric acid, the ilmenite concentrate of in terms of titanium dioxide about 14%, remaining is shale mineral, pyroxene, magnesium aluminate spinel, hornblend, green mud
Stone, olivine, quartz, magnetic iron ore and pyrite etc., owing to titaniferous amount is low, complicated component, it is impossible to directly return acidolysis workshop section
Utilize, stack generally as solid waste.Along with the expansion of domestic titanium white production business's production capacity, ilmenite concentrate resource is more and more precious
Expensive, arbitrarily stack not only waste resource and be also easy to cause environmental pollution.Inventor place company often produces one ton of titanium dioxide and i.e. produces
Raw 500 kilograms of acidolysis slags, calculate by producing 200000 tons of titanium dioxides per year, and within 1 year, acidolysis slag reaches 100,000 tons, the ambient pressure faced and heap
Field expropriation of land pressure is huge.
If reclaiming ilmenite concentrate therein and soluble titanium liquid by processed, within 1 year, titanium dioxide 10,000 can be reclaimed
More than 7000 tons, economic benefit and social benefit are notable.The most existing part producer gradually starts to pay attention to the recycling of acidolysis slag,
Titanium dioxide acid hydrolysis residue is reclaimed as the patent of publication number CN101469367A uses water to roughly select the method with magnetic separation；Publication number
The patent document of CN101161353A reports a kind of method that sulfate process titanium dioxide acidolysis waste material obtains ilmenite concentrate by flotation；Open
Number disclose for the patent of CN102602990A and a kind of to utilize the composition of different densities in hydrocyclone separation acidolysis slag, thus time
The method receiving acidolysis slag.These methods have a common feature, and it is all use various means by acidolysis slag useless
Impurity component separates, and finally obtains the slag of Ti content enrichment, we term it the selected slag of acidolysis, with the acidolysis essence that will obtain
Select slag to be sent to hydrolysis procedure and send into acidolysis pot participation acidolysis reaction together with causing water.
By experiment it was found that the selected slag of acidolysis that directly will obtain adds acidolysis in acidolysis pot, acidolysis rate up to
About 95%, but titaniferous composition therein is still without well being utilized, because the acidolysis using above method to obtain is selected
Often containing more coarse granule breeze in slag, this coarse granule breeze is difficult to participate in acidolysis reaction, can be deposited on the contrary in system
Vicious cycle, cumulative reduction acidolysis rate and production efficiency.Although using in the patent of Publication No. CN101469367A
First acidolysis slag is smashed the method with magnetic separation of roughly selecting that carries out again adding water and prepares the selected slag of acidolysis, but due to the composition of acidolysis slag
Complexity, ilmenite concentrate content is only about 14%, and remaining material hardness is uneven, and shale mineral are easy to ilmenite concentrate granule is formed bag
Cover, the selected slag of acidolysis finally obtained also cannot be made to have thinner fineness even if having carried out pulverizing, technique can be caused on the contrary
Loaded down with trivial details numerous and jumbled.The most in this scenario, acidolysis slag is smashed also it is only used to conveniently roughly select and the operation of magnetic separation.Additionally
It was also found that the selected slag of acidolysis owing to generally yielding has bigger viscosity, along with the carrying out of acidolysis reaction, the acid of generation
The selected cinder ladle of acidolysis of non-acidolysis can gradually be wrapped by hydrolysis products, causes middle unreacted material to be difficult to acidolysis, acidolysis
Rate therefore suffers from impact.
The recoverying and utilizing method of a kind of sulfuric acid method titanium pigment acidolysis slag mentioned by the present invention, is not the most shown in
To relevant open report.
Summary of the invention
For improving the utilization rate to acidolysis slag further, improve the acidolysis rate of the selected slag of gained acidolysis, the invention provides
A kind of recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag.
The technical solution adopted in the present invention is: the recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag, including following step
Rapid:
A, by acidolysis slag by selected raising Ti content, obtain the selected slag of acidolysis；
B, by selected for acidolysis slag add wet ball mill levigate；
C, levigate acidolysis slag filter pressing is dried up, obtain filter press cake；
D, addition sulphuric acid pump into acidolysis pot together with acidolysis ilmenite concentrate premix material mix making beating with filter press cake after and carry out acidolysis.
The present invention is levigate by the selected slag of acidolysis of selected gained adds wet ball mill, is converted by coarse granule breeze therein
For fine grained breeze, it is to avoid coarse granule breeze is difficult to participate in acidolysis reaction, is deposited on vicious cycle in system.To obtain simultaneously
Filter press cake is pulled an oar after mixing with sulphuric acid, it is therefore an objective to make that acidolysis selected slurry material is fully dispersed to be opened, it is to avoid follow-up acidolysis reaction
Unreacted material is wrapped by the acid hydrolysate of middle generation, the problem hindering acidolysis reaction to proceed, and improves acidolysis with this
The acidolysis rate of selected slag, uses the purpose of sulphuric acid mixing making beating to be the premix realizing sulphuric acid with slurry, it is simple to follow-up acidolysis is anti-
The carrying out answered, additionally can by regulation pull an oar used by sulfuric acid concentration, make used by sulfuric acid concentration in slurry and acidolysis reaction
Sulfuric acid concentration mates, it is to avoid use the impact on acid hemolysis process acid ore deposit ratio that water making beating causes.
As a further improvement on the present invention, described step A specifically comprises the processes of:
(1) the acidolysis slag that filter pressing workshop section produces is transported in hollander tub mix with water making beating, forms solid formation content 10
～the float slurry of 50%, send into dashpot standby；
(2) use the composition of hydrocyclone separation different densities, be acidolysis essence from hydrocyclone sand mouth material out
Select slag；Containing substantial amounts of titanyl sulfate in filtrate, collect Hou Songzhu acidolysis workshop section and do leaching water, with recovery Pd resource.
The program uses hydraulic cyclone technology, utilizes different components density variation recovery Pd concentrate, in removal process not
Introduce new impurity, it is to avoid new pollution, while recovery Pd concentrate, also reclaim soluble titanium.The mesh of making beating in the program
Be form uniform suspended nitride, in order to hydrocyclone, it is separated.
As a further improvement on the present invention, the selected slag of acidolysis described in step B breeze particle diameter after levigate is less than 45 μm
Granule in total particle proportion between 85～90%.It is demonstrated experimentally that in acidolysis selected slag particle footpath less than 45 μm
Granule is time in total particle, proportion reaches more than 90%, along with the increase of ball milling polishing time, the further reduction of fineness
And inconspicuous, and this ratio below 85% time, the selected slag of acidolysis also remains more be difficult to participate in acidolysis reaction thick
Granule breeze.
As a further improvement on the present invention, in step D, sulphuric acid is 1.5:1～2.5:1 with the liquid-solid ratio of filter press cake, to protect
Card making beating disposed slurry can scatter well.
As a further improvement on the present invention, after in step D, making beating terminates, the mass concentration of sulphuric acid is 53～57%.Mesh
The sulfuric acid concentration being to ensure that in making beating disposed slurry and the sulfuric acid concentration of acidolysis reaction match, to maintain the sour ore deposit of acid hemolysis process
Ratio, prevents exothermic heat of reaction not enough or thermal discharge is excessive exceedes suitable temperature range, reduces acidolysis rate.
As a further improvement on the present invention, the acidolysis selected slag TiO described in step A2Mass fraction is more than 40%, always
Weight of iron mark is more than 25%, and particle diameter is less than 50% less than the granule proportion of 45 μm.
As a further improvement on the present invention, in step C, time of filter pressing is 0.5～2h, and in filter cake, moisture content is little
In 20%.
As a further improvement on the present invention, the slurry after the making beating in step D and the ratio of acidolysis ilmenite concentrate premix material
For butt mass ratio 1:30～2:30.
The invention has the beneficial effects as follows: 1) improve acidolysis slag acidolysis rate；2) coarse granule breeze in the selected slag of acidolysis is avoided
The vicious cycle because of acidolysis effect difference, causes production efficiency to decline；3) use hydraulic cyclone technology, do not introduce in removal process
New impurity, it is to avoid new pollution, has also reclaimed soluble titanium while recovery Pd concentrate；4) fully Resource recovery, minimizing
Debris dump is high-volume.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
The present embodiment is used for illustrating the sulfuric acid process acidolysis selected slag wet grinding Application way of the present invention.
Selected for acidolysis slag (particle diameter is 50% more than 45 μm proportions) is levigate to shared by 45 μm by wet ball mill
Ratio is 85%, and then filter pressing filter cake uses the liquid-solid ratio of 1.5:1 mix making beating with sulphuric acid, sulfuric acid concentration 55% after making beating,
Then acidolysis pot acidolysis is pumped into together with acidolysis premix material.
Embodiment 2
The present embodiment is used for illustrating the sulfuric acid process acidolysis selected slag wet grinding Application way of the present invention.
Selected for acidolysis slag (particle diameter is 55% more than 45 μm proportions) is levigate to shared by 45 μm by wet ball mill
Ratio is 90%, and then filter pressing filter cake uses the liquid-solid ratio of 2.5:1 mix making beating with sulphuric acid, sulfuric acid concentration 57% after making beating,
Then acidolysis pot acidolysis is pumped into together with acidolysis premix material.
Embodiment 3
The present embodiment is used for illustrating the sulfuric acid process acidolysis selected slag wet grinding Application way of the present invention.
Selected for acidolysis slag (particle diameter is 55% more than 45 μm proportions) is levigate to shared by 45 μm by wet ball mill
Ratio is 90%, and then filter pressing filter cake uses the liquid-solid ratio of 1.5:1 mix making beating with sulphuric acid, sulfuric acid concentration 53% after making beating,
Then acidolysis pot acidolysis is pumped into together with acidolysis premix material.
Comparative example 1
This comparative example is used for contrasting the sulfuric acid process acidolysis selected slag wet grinding Application way of the present invention.
Selected for acidolysis slag (particle diameter is 55% more than 45 μm proportions) is pumped into acidolysis pot acid together with acidolysis premix material
Solve.
Comparative example 2
This comparative example is used for contrasting the sulfuric acid process acidolysis selected slag wet grinding Application way of the present invention.
Selected for acidolysis slag (particle diameter is 50% more than 45 μm proportions) is pumped into acidolysis pot acid together with acidolysis premix material
Solve.
| Numbering | Acidolysis rate % |
| Embodiment 1 | 97.88 |
| Embodiment 2 | 97.62 |
| Embodiment 3 | 97.77 |
| Comparative example 1 | 95.12 |
| Comparative example 2 | 94.87 |
According to embodiment and comparative example, the method using the present invention, by levigate for selected for acidolysis slag wet ball mill to being less than
45 μm proportions between 85～90%, then filter pressing, then pull an oar with liquid-solid ratio 1.5～2.5:1, it is ensured that after making beating
Sulfuric acid concentration 53～57%, the method pumping into acidolysis pot acidolysis afterwards together with premix material.Acidolysis rate ratio is without above-mentioned steps
And be pumped directly into acidolysis pot acidolysis and all improve a lot.By the inventive method, both improve the acidolysis rate of acidolysis slag, the most permissible
Avoiding the coarse granule breeze vicious cycle of acidolysis effect difference in the selected slag of acidolysis, the most simple to operate, equipment investment is few, has relatively
Big economic benefit.
Claims (8)
1. the recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag, comprises the following steps:
A, by acidolysis slag by selected raising Ti content, obtain the selected slag of acidolysis；
It is characterized in that: also include step B, step C and step D, particularly as follows:
B, by selected for acidolysis slag add wet ball mill levigate；
C, levigate acidolysis slag filter pressing is dried up, obtain filter press cake；
D, addition sulphuric acid pump into acidolysis pot together with acidolysis ilmenite concentrate premix material mix making beating with filter press cake after and carry out acidolysis.
The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag the most according to claim 1, it is characterised in that: described step
A's specifically comprises the processes of:
(1) the acidolysis slag that filter pressing workshop section produces is transported in hollander tub mix making beating with water, formation solid formation content 10～
The float slurry of 50%, sends into dashpot standby；
(2) use the composition of hydrocyclone separation different densities, be the selected slag of acidolysis from hydrocyclone sand mouth material out；
Containing substantial amounts of titanyl sulfate in filtrate, collect Hou Songzhu acidolysis workshop section and do leaching water, with recovery Pd resource.
The recoverying and utilizing method of sulfuric acid method titanium pigment acidolysis slag the most according to claim 1, it is characterised in that: in step B
The selected slag of described acidolysis after levigate breeze particle diameter less than the granule of 45 μm in total particle proportion between 85～90% it
Between.
4. according to the recoverying and utilizing method of the sulfuric acid method titanium pigment acidolysis slag described in claim 1 or 3, it is characterised in that: step D
Middle sulphuric acid is 1.5:1～2.5:1 with the liquid-solid ratio of filter press cake.
5. according to the recoverying and utilizing method of the sulfuric acid method titanium pigment acidolysis slag described in claim 1 or 3, it is characterised in that: step D
After middle making beating terminates, the mass concentration of sulphuric acid is 53～57%.
6. according to the recoverying and utilizing method of the sulfuric acid method titanium pigment acidolysis slag described in claim 1 or 3, it is characterised in that: step A
Described in acidolysis selected slag TiO2Mass fraction be more than 40%, total weight of iron mark be more than 25%, particle diameter less than 45 μm
Grain proportion is less than 50%.
7. according to the recoverying and utilizing method of the sulfuric acid method titanium pigment acidolysis slag described in claim 1 or 3, it is characterised in that: step C
Middle time of filter pressing is 0.5～2h, and in filter cake, moisture content is less than 20%.
8. according to the recoverying and utilizing method of the sulfuric acid method titanium pigment acidolysis slag described in claim 1 or 3, it is characterised in that: step D
In making beating after the ratio of slurry and acidolysis ilmenite concentrate premix material be butt mass ratio 1:30～2:30.
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| CN108726563A (en) * | 2018-06-08 | 2018-11-02 | 龙蟒佰利联集团股份有限公司 | A kind of method that acidolysis tailing recycles in production process of titanium pigment |
| CN111495517A (en) * | 2020-04-22 | 2020-08-07 | 龙佰四川钛业有限公司 | Hydrolysis scale depolymerization method |
| CN114377860A (en) * | 2021-12-06 | 2022-04-22 | 宜宾天原海丰和泰有限公司 | Resource utilization method of titanium dioxide chlorination dust collection slag by chlorination process |
| CN115536061A (en) * | 2022-11-04 | 2022-12-30 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate from low-grade titanium ore |
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| CN106745232A (en) * | 2017-02-24 | 2017-05-31 | 四川龙蟒钛业股份有限公司 | A kind of recoverying and utilizing method for hydrolyzing dirt |
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| CN107413521A (en) * | 2017-04-25 | 2017-12-01 | 潜江方圆钛白有限公司 | The industrial method of magnetic separation ilmenite concentrate in acidolysis tailings is produced from sulfuric acid method titanium pigment |
| CN108726563A (en) * | 2018-06-08 | 2018-11-02 | 龙蟒佰利联集团股份有限公司 | A kind of method that acidolysis tailing recycles in production process of titanium pigment |
| CN111495517A (en) * | 2020-04-22 | 2020-08-07 | 龙佰四川钛业有限公司 | Hydrolysis scale depolymerization method |
| CN114377860A (en) * | 2021-12-06 | 2022-04-22 | 宜宾天原海丰和泰有限公司 | Resource utilization method of titanium dioxide chlorination dust collection slag by chlorination process |
| CN114377860B (en) * | 2021-12-06 | 2024-03-01 | 宜宾天原海丰和泰有限公司 | Resource utilization method for chloridized dust collection slag of titanium dioxide by chloridizing method |
| CN115536061A (en) * | 2022-11-04 | 2022-12-30 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate from low-grade titanium ore |
| CN115536061B (en) * | 2022-11-04 | 2024-01-26 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate from low-grade titanium ore |
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