CN109250751A - Handle the method that titanium tetrachloride purification removes vanadium mud - Google Patents
Handle the method that titanium tetrachloride purification removes vanadium mud Download PDFInfo
- Publication number
- CN109250751A CN109250751A CN201811258519.4A CN201811258519A CN109250751A CN 109250751 A CN109250751 A CN 109250751A CN 201811258519 A CN201811258519 A CN 201811258519A CN 109250751 A CN109250751 A CN 109250751A
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- CN
- China
- Prior art keywords
- titanium tetrachloride
- mud
- vanadium
- vanadium mud
- ore pulp
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
Abstract
The invention belongs to titanium field of metallurgy, and in particular to a method of processing titanium tetrachloride purification removes vanadium mud.Technical problem to be solved by the invention is to provide a kind of methods that the purification of processing titanium tetrachloride removes vanadium mud, comprising the following steps: a, refines titanium tetrachloride except vanadium mud is concentrated, obtains dense ore pulp；B, dense ore pulp is put into the dust collecting system of fused salt chlorimation process, titanium tetrachloride gasification enters fused salt chlorimation flue gas in dense ore pulp.The method of the present invention can refine titanium tetrachloride except the TiCl in vanadium mud4It recycles.
Description
Technical field
The invention belongs to titanium field of metallurgy, and in particular to a method of processing titanium tetrachloride purification removes vanadium mud.
Background technique
Titanium tetrachloride is the important intermediate products for producing Titanium and its titanium compound, is the important original of Ti industry production
Material is widely used in the industries such as production Titanium, titanium white, titanium trichloride.Thick TiCl4It is to be produced using titanium-riched material chlorination production, nothing
By be fluidizing chlorination or fused salt chlorimation production crude titanic chloride in all there are many objectionable impurities, pass through distillation, rectifying side
Method can remove the high and low boiling contaminants in crude titanic chloride, by chemical method such as aluminium powder except vanadium method, organic matter are except the removing such as vanadium method
Foreign matter of vanadium in titanium tetrachloride.
A large amount of titanium tetrachloride mud containing vanadium, especially aluminium powder can be generated except vanadium is raw by removing in above-mentioned purification in vanadium production process
It is generated in production and contains VOCl2The titanium tetrachloride mud of equal solid impurities, mud amount accounts for about the 1/10 of titanium tetrachloride product volume, due to four
Titanium chloride mud yield is big, if do not recycled, will cause a large amount of losses of titanium tetrachloride.At present for aluminium powder except vanadium produces
The raw processing method of titanium tetrachloride mud containing vanadium removes Al first is that first settling using hydrolysis, and pulp vaporizing furnace is recycled to carry out
TiCl4Recycling, remaining residue containing vanadium add lime neutralisation treatment.This method treatment process control process is cumbersome, and ore pulp evaporates heel row
Environmental pollution is serious when slag, not high to the recovery utilization rate of titanium tetrachloride.
CN102009999A, which is disclosed, handles titanium tetrachloride mud using paddle-dryer, avoids using hydrolysis process
As hydrolysis control it is improper and caused by the method lost of titanium tetrachloride, but its essence is still that a kind of external heat mud makes wherein
TiCl4Be evaporated the process separated.But aluminium powder is larger except the vanadium slag mud amount that vanadium generates, and such processing method uses
Steam source, titanium tetrachloride mud heating temperature are only 140 DEG C~148 DEG C, and the efficiency of processing is very low, according to 15kt/a's
Titanium sponge business accounting, the yield for refining mud reach 20t or more daily, it is difficult to meet the production fortune under high-load condition
Row.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of methods that the purification of processing titanium tetrachloride removes vanadium mud.The party
Method the following steps are included:
A, titanium tetrachloride purification is obtained into dense ore pulp except vanadium mud is concentrated；
B, dense ore pulp is put into the dust collecting system of fused salt chlorimation process, titanium tetrachloride gasification enters fused salt chlorine in dense ore pulp
Change flue gas.
Specifically, above-mentioned processing titanium tetrachloride purification is except in the method and step a of vanadium mud, the titanium tetrachloride purification removes vanadium
Mud refers to the crude titanic chloride mud that pressure bottoms discharges after aluminium powder is except vanadium.
Specifically, above-mentioned processing titanium tetrachloride purification removes in the method and step a of vanadium mud, it is described to be concentrated into the 1/ of original volume
3~2/3.
Further, the purification of above-mentioned processing titanium tetrachloride is except in the method and step a of vanadium mud, the original volume that is concentrated into
1/2。
Preferably, the purification of above-mentioned processing titanium tetrachloride except in the method and step b of vanadium mud, control the flue gas of dust collecting system into
Mouth temperature is 250~300 DEG C, and flue gas exit temperature is 150~180 DEG C.
Specifically, above-mentioned processing titanium tetrachloride purification is except in the method and step b of vanadium mud, the dust collecting system is second
Grade dust collecting system.
The method of the present invention is using fused salt chlorimation process to except the TiCl in vanadium mud4It is recycled, on the one hand can reduce biography
Ore pulp evaporation technology process in technique of uniting saves the heating power consumption being additionally required when ore pulp evaporation and processing time；Another party
Face can solve a large amount of TiCl that traditional handicraft is faced when ore pulp evaporates deslagging4The problems such as flue gas, bad environments, environmental protection pressure.
The present invention makes mud realize TiCl under the spray condition that gasifies using chlorination furnace flue gas heat4It efficiently separates, obtained dust-slag collection
Under traditional handicraft processing mode, do not increase environmentally friendly risk additionally.The method of the present invention not only saves energy, and right
TiCl4The rate of recovery than conventional method increase by 3% or more.
Specific embodiment
The present invention handles the method that titanium tetrachloride purification removes vanadium mud, comprising the following steps:
A, aluminium powder is obtained into the dense ore pulp of 1/3~2/3 amount except the purification mud containing vanadium after vanadium carries out sedimentation concentration processing；
B, the dense ore pulp obtained after concentration is pumped into the dust collecting system of fused salt chlorimation process；Dense ore pulp returns to dust collecting system
Afterwards, dust collecting system flue-gas temperature is controlled, makes inlet temperature control at 250 DEG C~300 DEG C, exit gas temperature is controlled at 150 DEG C
~180 DEG C；Make most TiCl in mud by controlling temperature4Gasification enters in fused salt chlorimation flue gas, allows VOCl in mud2
And AlCl3Enter in dust-slag collection in solid form, to realize purification except the recycling of titanium tetrachloride in vanadium mud.
The method of the present invention step b is passed through the flue gas of dust collecting system by fused salt chlorimation process, and (the practical flue gas is fused salt chlorine
The titanium tetrachloride product clip hetero moiety impurity of chemical industry sequence) heating and gasifying is carried out to the dense ore pulp that dust collecting system is added, make dense ore pulp
In titanium tetrachloride gasification, dust collecting system is scrubbed, condensing mode processing for discharge after the two mixing, make titanium tetrachloride smoke by
Step is cooled to titanium tetrachloride liquid, collects, subsequently into refining system.
In the method for the present invention step b, if dust collecting system flue-gas temperature is excessively high, TiCl4Middle Fe, Al impurity is more, except after vanadium
Solid phase VOCl2Disproportionated reaction can occur and regenerate VOCl3In TiCl4Middle enrichment；If dust collecting system flue-gas temperature is too low,
Even below TiCl4Boiling point will lead to TiCl4Into the slag ladle that gathers dust, elution cannot be normally entered and be collected, dust collecting system meeting
Occur largely containing TiCl4Solvent or diluent.It is 250~300 DEG C it is advantageous to the gas inlet temperature of dust collecting system.The cigarette of dust collecting system
Gas outlet temperature is 150~180 DEG C.By control inlet and outlet, the function of dust collecting system is realized, it is excessively high or too low
It is unfavorable.
In the method for the present invention step b, the cooling dust collection capacity of dust collecting system be it is certain, in normal chlorination furnace working condition
Under, the temperature by control inlet and outlet is unique control parameter that it realizes function, the flux matched ability of the amount of flue gas and dense ore pulp
It is able to satisfy temperature controlling range, in other words, such as dense ore pulp amount to be treated is excessive, then is unable to control dust collecting system import temperature
Degree is 250~300 DEG C, outlet temperature is 150~180 DEG C.
Embodiment 1
The VOCl obtained after western high calcium magnesium titanium slag fused salt chlorimation will be climbed3Thick TiCl of the content 0.18%4, it is added to distillation
In kettle, while previously prepared TiCl is added3Ore pulp is (by Al powder and TiCl4, it is passed through a small amount of Cl2It is made), the chemistry of generation is anti-
It answers:
Al(s)+TiCl4(l)+Cl2(g)→TiCl3(s)+AlCl3(s、l)
VOCl3(l)+TiCl3(s)→VOCl2(s)↓+TiCl4(l)
Residue after aluminium powder is except vanadium is discharged from distillation still bottom, then will settle except the purification mud containing vanadium after vanadium
Concentration obtains the dense ore pulp of 1/2 amount, and the dense ore pulp obtained after concentration is got to surge tank before chlorination furnace by submerged pump
In, then by the second level dust collecting system of revert system and nozzle one chlorination furnace of return, control dust collecting system flue-gas temperature, make
At 280 DEG C, exit gas temperature is controlled at 180 DEG C for inlet temperature control.Make most TiCl in mud by controlling temperature4
Gasification enters in fused salt chlorimation flue gas, allows VOCl in mud2And AlCl3Enter in dust-slag collection in solid form, dust-slag collection is taken to detect
It was found that wherein containing a large amount of VOCl2And AlCl3, while obtained thick TiCl4Middle VOCl3Content still can control
0.18% hereinafter, not to thick TiCl4Quality impacts, while the treating capacity of pulp vaporizing furnace reduces 1/3, realizes that purification removes
TiCl in vanadium mud4Recycling, reduce the treating capacity of pulp vaporizing furnace.
Embodiment 2
By VOCl after blast furnace slag high temperature cabonization-low temperature chlorination3Thick TiCl of the content 0.3%4, it is incorporated according to a certain percentage
VOCl3Thick TiCl of the content 0.15%4, it is added in distillation still, while previously prepared TiCl is added3Ore pulp (by Al powder with
TiCl4, it is passed through a small amount of Cl2It is made), the chemical reaction of generation:
Al(s)+TiCl4(l)+Cl2(g)→TiCl3(s)+AlCl3(s、l)
VOCl3(l)+TiCl3(s)→VOCl2(s)↓+TiCl4(l)
Residue after aluminium powder is except vanadium is discharged from distillation still bottom, then will settle except the purification mud containing vanadium after vanadium
Concentration obtains the dense ore pulp of 1/2 amount, and the dense ore pulp obtained after concentration is got to surge tank before chlorination furnace by submerged pump
In, then by the second level dust collecting system of revert system and nozzle one chlorination furnace of return, control dust collecting system flue-gas temperature, make
At 260 DEG C, exit gas temperature is controlled at 160 DEG C for inlet temperature control.Make most TiCl in mud by controlling temperature4
Gasification enters in fused salt chlorimation flue gas, allows VOCl in mud2And AlCl3Enter in dust-slag collection in solid form, dust-slag collection is taken to detect
It was found that wherein containing a large amount of VOCl2And AlCl3, while obtained thick TiCl4Middle VOCl3Content still can control 0.2%
Hereinafter, not to thick TiCl4Quality impacts, while the treating capacity of pulp vaporizing furnace substantially reduces, and realizes that purification removes vanadium mud
Middle TiCl4Recycling, reduce the treating capacity of pulp vaporizing furnace.
Claims (6)
1. handling the method that titanium tetrachloride purification removes vanadium mud, it is characterised in that: the following steps are included:
A, titanium tetrachloride purification is obtained into dense ore pulp except vanadium mud is concentrated；
B, dense ore pulp is put into the dust collecting system of fused salt chlorimation process, titanium tetrachloride gasification enters fused salt chlorimation cigarette in dense ore pulp
Gas.
2. the method that processing titanium tetrachloride purification according to claim 1 removes vanadium mud, it is characterised in that: in step a, institute
Titanium tetrachloride purification is stated except vanadium mud refers to the crude titanic chloride mud that pressure bottoms discharges after aluminium powder is except vanadium.
3. the method that processing titanium tetrachloride purification according to claim 1 removes vanadium mud, it is characterised in that: in step a, institute
It states and is concentrated into the 1/3~2/3 of original volume.
4. the method that processing titanium tetrachloride purification according to claim 3 removes vanadium mud, it is characterised in that: in step a, institute
It states and is concentrated into the 1/2 of original volume.
5. the method that processing titanium tetrachloride purification according to claim 1 removes vanadium mud, it is characterised in that: in step b, control
The gas inlet temperature of dust collecting system processed is 250~300 DEG C, and flue gas exit temperature is 150~180 DEG C.
6. the method that processing titanium tetrachloride purification according to claim 1 removes vanadium mud, it is characterised in that: in step b, institute
The dust collecting system stated is second level dust collecting system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811258519.4A CN109250751A (en) | 2018-10-26 | 2018-10-26 | Handle the method that titanium tetrachloride purification removes vanadium mud |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811258519.4A CN109250751A (en) | 2018-10-26 | 2018-10-26 | Handle the method that titanium tetrachloride purification removes vanadium mud |
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| CN109250751A true CN109250751A (en) | 2019-01-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111422900A (en) * | 2020-04-28 | 2020-07-17 | 攀钢集团钛业有限责任公司 | Vanadium-removing slurry treatment device and process |
| CN115821071A (en) * | 2022-12-13 | 2023-03-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium tetrachloride vanadium-removing slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415547A (en) * | 2002-07-19 | 2003-05-07 | 锦州铁合金(集团)股份有限公司钛白粉厂 | Technique and method for treating titanium tetrachloride slurry containing vanadium |
| CN106853985A (en) * | 2015-12-08 | 2017-06-16 | 云南冶金新立钛业有限公司 | Method of the treatment containing vanadium mud |
-
2018
- 2018-10-26 CN CN201811258519.4A patent/CN109250751A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415547A (en) * | 2002-07-19 | 2003-05-07 | 锦州铁合金(集团)股份有限公司钛白粉厂 | Technique and method for treating titanium tetrachloride slurry containing vanadium |
| CN106853985A (en) * | 2015-12-08 | 2017-06-16 | 云南冶金新立钛业有限公司 | Method of the treatment containing vanadium mud |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111422900A (en) * | 2020-04-28 | 2020-07-17 | 攀钢集团钛业有限责任公司 | Vanadium-removing slurry treatment device and process |
| CN115821071A (en) * | 2022-12-13 | 2023-03-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Treatment method of titanium tetrachloride vanadium-removing slurry |
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Application publication date: 20190122 |