CN108585034A - The method that ilmenite prepares high-strength artificial rutile - Google Patents
The method that ilmenite prepares high-strength artificial rutile Download PDFInfo
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- CN108585034A CN108585034A CN201810785059.4A CN201810785059A CN108585034A CN 108585034 A CN108585034 A CN 108585034A CN 201810785059 A CN201810785059 A CN 201810785059A CN 108585034 A CN108585034 A CN 108585034A
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- Prior art keywords
- ilmenite
- strength artificial
- leaching
- rutile
- artificial rutile
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- Granted
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 78
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000002386 leaching Methods 0.000 claims abstract description 46
- 230000009467 reduction Effects 0.000 claims abstract description 33
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000007790 solid phase Substances 0.000 claims description 23
- 238000006213 oxygenation reaction Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 18
- 230000001590 oxidative effect Effects 0.000 claims description 14
- 238000009826 distribution Methods 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000005065 mining Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 150000007529 inorganic bases Chemical class 0.000 claims description 7
- 150000007522 mineralic acids Chemical class 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 239000010936 titanium Substances 0.000 abstract description 9
- 238000010405 reoxidation reaction Methods 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 5
- 238000010410 dusting Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910052719 titanium Inorganic materials 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 230000009257 reactivity Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 36
- 230000008569 process Effects 0.000 description 21
- 239000012530 fluid Substances 0.000 description 17
- 239000007787 solid Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
- 238000005660 chlorination reaction Methods 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012795 verification Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C01G23/0475—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods that ilmenite prepares high-strength artificial rutile, belong to metallurgical technology field.The present invention is in order to solve the problems, such as that existing synthetic rutile intensity is low, easy dusting, provide a kind of method that ilmenite prepares high-strength artificial rutile, ilmenite obtains synthetic rutile through " the weak reduction high temperature reoxidation acidleach alkali leaching calcining of high-temperature oxydation ".The method of the present invention changes the microcosmic composition of ilmenite and form by carrying out " the weak reduction high temperature reoxidation of high-temperature oxydation " pretreatment to ilmenite, make it during follow-up acidleach alkali leaching is miscellaneous while there is good reactivity and resistance to mechanical power, make titanium recovery rate up to 98% or more, product quality is high, TiO2Content higher, granularity keep more preferable, and fine powder ratio is lower.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a kind of method that ilmenite prepares high-strength artificial rutile.
Background technology
Fluidizing chlorination titanium white is the development trend of current world's titanium white industry.Compared to sulfate process titanium dioxide, it is more advanced, but
It is but more harsh to ingredient requirement.The ilmenite titanium resource most abundant as reserves in the world is higher due to largely having
The impurity such as iron, calcium, magnesium, the silicon of content cannot be directly used as fluidizing chlorination raw material, all to be typically necessary upgrading processing.Therefore,
It is always the development priority in titanium industry field preparing fluidizing chlorination with synthetic rutile raw material using ilmenite as raw material.
Proposed it is a variety of synthetic rutile method prepared as raw material using ilmenite, hydrochloric acid leaching process is due to its height
The advantages such as the dust removal rate of effect and sour recoverable, it is most promising.By Benilite companies of the U.S. in patent
The pre- weak reduction-hydrochloric acid pressure leaching process put forward in US3967954 is the hydrochloric acid method technique being used widely early stage；But
Being it must use high-grade ilmenite placer for raw material, and otherwise dust removal rate is not high.On the basis of BCA, researcher carries again
The weak reduction of Strong oxdiative-- hydrochloric acid leaching process technique, such as patent US4097574, US5885324, CN201010276812 are gone out
Deng these techniques are stronger to adaptability to raw material, dust removal rate higher, can handle that rate of decay is different, grade is different simultaneously
Various ilmenites；But the problem of these techniques are there is also product dusting, and granularity is unsatisfactory for follow-up fluidizing chlorination requirement.
There is researcher to notice this problem, is proposed in patent CN201310534032 pre- by the weak reduction of Strong oxdiative-in ilmenite
After processing, using the Leaching way of fluid bed, to reduce the agitation during acidleach, this method greatly reduces acidleach really
Dusting in the process, most of product maintain original particle size；But there is no occur for redox pretreatment and acidleach process
Essential change, therefore, this method do not change the low essence of synthetic rutile product strength, and product once applies to subsequently belong to
During the fluidizing chlorination of dense gas solid bed, strong particles collision will cause the dusting again of synthetic rutile raw material,
To cause chlorination process titanium yield to be greatly reduced, dust pelletizing system pressure aggravate the problems such as.
Invention content
The problem of that the technical problem to be solved by the present invention is to the synthetic rutile intensity of prior art production is low, easy dusting.
The present invention solves technical solution used by above-mentioned technical problem, and there is provided a kind of ilmenites to prepare high intensity people
The method for making rutile comprising following steps：
A, the oxidized roasting of ilmenite obtains the oxide ore of oxygenation efficiency >=80%；
B, oxide ore obtained by step A obtains the reduced ore of reduction rate >=80% in reducing atmosphere through reduction roasting；
C, the oxidized roasting of reduced ore obtained by step B, obtain oxygenation efficiency >=50% reoxidizes mine；
D, mining inorganic Ore Leaching is reoxidized obtained by step C, solid-liquor separation must leach solid phase；
E, solid phase is leached obtained by step D to be leached with inorganic alkali solution, through solid-liquor separation, washing, obtain synthetic rutile first product,
First product obtains high-strength artificial rutile through calcining.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step A, the ilmenite
In the TiO containing 40~60 weight %2With the SiO of 1~8 weight %2。
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step A, the ilmenite
Size distribution be 60~200 mesh.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step A, the oxidation roasting
The temperature of burning is 850~1050 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step A, the oxidation roasting
The time of burning is 0.5~2h.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step B, the reduction roasting
The temperature of burning is 700~800 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step B, the reduction roasting
The time of burning is 0.5~4h.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step C, the oxidation roasting
The temperature of burning is 850~1050 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step C, the oxidation roasting
The time of burning is 0.2~0.5h.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, the inorganic acid
For hydrochloric acid or sulfuric acid.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, the inorganic acid
A concentration of 15~25 weight %.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, the hydrochloric acid with
The volume mass ratio for reoxidizing mine is 3~4：1.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, inorganic Ore Leaching
When, control mixing speed is 200~500r/min.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, the leaching
Temperature is 80~105 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step D, the leaching
Time is 2~6h.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the inorganic base
For NaOH or KOH.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the inorganic base
A concentration of 5~15 weight % of solution.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the inorganic base
Solution is 1~3 with the volume mass ratio for leaching solid phase：1.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the leaching
Temperature is 30~80 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the leaching
Time is 0.5~1h.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the calcining
Temperature is 300~700 DEG C.
Wherein, ilmenite described above is prepared in the method for high-strength artificial rutile, in step E, the calcining
Time is 0.2~1h.
In the method for the present invention, the oxygenation efficiency indicates (trivalent Fe contents/total Fe contents) × 100%, the reduction rate table
Show (1- trivalent Fe contents/total Fe contents) × 100%.
Heretofore described volume mass ratio be liquid by volume, solid in mass, the two be with order of magnitude unit,
Example is when volume unit is L, mass unit kg.
The beneficial effects of the invention are as follows：
The method of the present invention changes ferrotianium by carrying out " the weak reduction-high temperature reoxidation of high-temperature oxydation-" pretreatment to ilmenite
The microcosmic composition of mine and form make it during follow-up acidic leaching with alkaline leaching is miscellaneous while having good reactivity and resistance to mechanical
Power makes titanium recovery rate up to 98% or more, and gained synthetic rutile intensity is high, TiO2Content higher, granularity keep more preferable, fine powder ratio
Example is lower, small for being lost when follow-up fluidizing chlorination.
The method of the present invention is adaptable to ilmenite raw material, and high temperature reoxidation process is autothermal reaction, and energy consumption is low, is taken
It is short, it is lower to equipment requirement, it can directly utilize existing equipment；It is simple for process, it is efficient, it is at low cost, it can be achieved that extensive continuous
Production.
Description of the drawings
Fig. 1 is the process flow diagram that ilmenite of the present invention prepares high-strength artificial rutile.
Specific implementation mode
The present invention is in fully research ilmenite in the reaction mechanism mechanism of reaction and changing rule of redox pretreatment and acidleach process
On the basis of, it is proposed that by high-strength to prepare with " the weak reduction-high temperature reoxidation of high-temperature oxydation-- acidic leaching with alkaline soaks " processing ilmenite
The production technology of synthetic rutile is spent, which includes the following steps：
A, the oxidized roasting of ilmenite obtains the oxide ore of oxygenation efficiency >=80%；
B, oxide ore obtained by step A obtains the reduced ore of reduction rate >=80% in reducing atmosphere through reduction roasting；
C, the oxidized roasting of reduced ore obtained by step B, obtain oxygenation efficiency >=50% reoxidizes mine；
D, mining salt Ore Leaching is reoxidized obtained by step C, solid-liquor separation must leach solid phase；
E, solid phase is leached obtained by step D to be leached with NaOH solution, through solid-liquor separation, washing, obtain synthetic rutile first product, just
Product obtain high-strength artificial rutile through calcining.
In the method for the present invention step A, the TiO containing 40~60 weight % in used ilmenite2With 1~8 weight %
SiO2, other main components are weight %, Fe of FeO25~402O3Weight %, CaO0~1.5 of 0~10 weight %, MgO0~8
Weight % and Al2O30~1.5 weight %；And since follow-up fluidizing chlorination process is distribution to the granularity requirements of synthetic rutile
Between 60-200 mesh, therefore it is 60~200 mesh that the present invention, which controls the size distribution of ilmenite, the final artificial gold for preparing gained
98% or more size distribution of red stone is between 60~200 mesh, and product granularity is kept, and fine powder ratio is low.
In the method for the present invention step A, oxidizing roasting is generally in air or oxygen atmosphere in fluid bed either rotary kiln
Middle progress, temperature are 850~1050 DEG C, and the time is 0.5~2h, to control oxygenation efficiency >=80% of gained oxide ore；Oxidation
Mine oxygenation efficiency is higher, and the active higher of sequential reduction roasting is conducive to control product quality.
In the method for the present invention step B, reduction roasting is generally in H in fluid bed or rotary kiln2(volume content is more than
20%) it or in the reducing atmosphere (such as coal gas or hydrogen) of CO (volume content is more than 30%) carrying out, temperature is 700~800 DEG C,
Time is 0.5~4h, to control reduction rate >=80% of gained reduced ore；Reduced ore reduction rate is higher, in ilmenite particle
Portion's hole is more, is conducive to subsequently to reoxidize and acidleach.
In the method for the present invention step C, oxidizing roasting is generally in fluid bed or rotary kiln in air or oxygen atmosphere
It carries out, temperature is 850~1050 DEG C, and the time is 0.2~0.5h, to control oxygenation efficiency >=50% of gained oxide ore；Oxygen again
Changing mainly makes to form TiO inside mineral grain2, oxygenation efficiency height is conducive to TiO2It generates, is conducive to protect during mineral grain acidleach
Hold high intensity；And the high temperature reoxidation process in step C is autothermal reaction, and energy consumption is low, is taken short.
In the method for the present invention step A~C, in order to energy saving, in " the weak reduction-high temperature reoxidation of high-temperature oxydation-" process,
The general material hot using loading is roasted.
The method of the present invention changes ilmenite by carrying out the weak reduction of high-temperature oxydation-- high temperature reoxidation pretreatment to ilmenite
Microcosmic composition and form make it during follow-up salt Ore Leaching-alkali leaching is miscellaneous while having good reactivity and anti-machine
Tool power.
In the method for the present invention step D, it is preferred to use the inorganic acid of a concentration of 15~25 weight % and reoxidize mine by volume
Mass ratio is 3~4：1 carries out acidleach；Wherein, the temperature of leaching is 80~105 DEG C, and the time of leaching is 2~6h；Acidleach is completed
Afterwards, it is separated by solid-liquid separation and obtains leaching solid phase and leachate；The leaching equipment of acidleach is needed using leaching ball or fluidisation with stirring
Bed etc., and mixing speed when controlling salt Ore Leaching reaches 200~500r/min, stirring is conducive to solid-liquid diffusion, improves and leach
Reaction rate.Wherein, inorganic acid can be hydrochloric acid or sulfuric acid；When using hydrochloric acid, hydrochloric acid, which can spray, to be recycled into regenerated acid,
And regenerated acid cycle is used for leaching process, realize acid cycle, but according to sulfuric acid, recycling cycle difficulty is big.
In the method for the present invention step E, it is preferred to use the inorganic alkali solution of a concentration of 5~15 weight % presses body with solid phase is leached
Product mass ratio is 1~3：1 leaching alkali leaching is miscellaneous；Wherein, the temperature of leaching is 30~80 DEG C, and the time of leaching is 0.5~1h；Alkali
Soaking technology makes synthetic rutile quality more primarily to remove Ca the and Si impurity in the silicic acid impuritiess that can not take out of acidleach
It is good；Wherein, inorganic base is NaOH or KOH；Alkali soaks step since reaction condition is relatively mild, and reacting dose is small, therefore alkali leaching pair is set
Standby and mixing speed requires not stringent.
It after the completion of alkali leaching, is separated by solid-liquid separation, gained solid phase is washed to get to synthetic rutile first product；When washing, in order to save
About cost can be washed first using leachate obtained by step D, be washed with water and wash, and removal is adsorbed on the foreign ion on solid
Deng；In step E, synthetic rutile first product is calcined 0.2~1 hour for 300~700 DEG C in rotary kiln, you can obtains high intensity people
Make rutile product.
Preferably, the method that ilmenite prepares high-strength artificial rutile, includes the following steps：
A, by ilmenite (TiO240~60 weight %, SiO21~8 weight %) fluid bed or revolution furnace air or
850~1050 DEG C of 0.5~2h of oxidizing roasting under oxygen atmosphere, obtain the oxide ore of oxygenation efficiency >=80%；
B, hot oxide ore is packed into lower one of fluid bed or rotary kiln, in H2(volume content be more than 20%) or
700~800 DEG C of 0.5~4h of reduction roasting in the reducing atmosphere of CO (volume content is more than 30%), obtain reduction rate >=80% also
Raw ore；
C, hot reduced ore is reloaded into down in one of fluid bed or rotary kiln, 850 under air or oxygen atmosphere~
1050 DEG C of 0.2~0.5h of oxidizing roasting, obtain oxygenation efficiency >=50% reoxidizes mine；
D, it is 3~4 that will reoxidize mining 15~25 weight % inorganic bases (hydrochloric acid or sulfuric acid) in liquid solid product mass ratio：1
(L/kg) under, control mixing speed is 200~500r/min, and 80~105 DEG C of 2~6h of normal pressure leaching, solid-liquor separation must leach solid
Phase and leachate；
E, it is 1~3 in liquid solid product mass ratio that will leach solid phase with 5~15 weight % inorganic bases (NaOH or KOH) solution：
Under 1 (L/kg), 30~80 DEG C of 0.5~1h of leaching, solid-liquor separation is washed with water after solid phase leachate obtained by step D washs
It washs, obtains synthetic rutile first product, first product 300~700 DEG C of 0.2~1h of calcining in rotary kiln obtain the production of high-strength artificial rutile
Product.
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
Embodiment 1
The present embodiment selects the main component of ilmenite：TiO2：46.76%, FeO：35.59%, Fe2O3：5.12%,
MgO：6.62%, CaO：1.03%, SiO2：4.56%, Al2O3：1.26%；Its size distribution is average between 60~200 mesh
Granularity is 185 μm；Specific preparation process is as follows：
A, by ilmenite in fluid bed 1000 DEG C of oxidizing roasting 1h under air atmosphere, obtain the oxidation that oxygenation efficiency is 95%
Mine；
B, by oxide ore in fluid bed 750 DEG C of reduction roasting 1h under coke-stove gas, obtain the reduction that reduction rate is 92%
Mine；
C, by reduced ore in fluid bed 1000 DEG C of oxidizing roasting 0.2h under air atmosphere, it is 87% again to obtain oxygenation efficiency
Oxide ore；
D, mining 20 weight % hydrochloric acid will be reoxidized in the reactor with strong mixing (rotating speed 500r/min), liquid is solid
Than 4：1 (L/kg), temperature are to leach 4h at 105 DEG C, are separated by solid-liquid separation, and obtain leaching solid phase and leachate, 98.5% or more is solid
For phase size distribution between 60~200 mesh, average particle size is 183 μm；
E, will leach solid phase with 8 weight %NaOH in liquid-solid ratio 2：1 (L/kg), temperature be 50 DEG C at leach 0.5h, Gu
After liquid separation, it is washed with water and washs 2 times after washing 1 time with the leachate of step D, obtain synthetic rutile first product, synthetic rutile
First product 500 DEG C of calcining 1h in rotary kiln, obtain high-strength artificial rutile product.
High-strength artificial rutile product obtained by the present embodiment, 98% or more size distribution are average between 60~200 mesh
Granularity is 183 μm, and main component is：TiO2：94.14%, FeO：2.15%, MgO：0.61%, CaO：0.11%, SiO2：
2.13%, Al2O3：The rate of recovery of 0.68%, whole process Ti are 98.5%；Verification test shows the product in cold conditions gas-solid flow
Change in bed and uses N22h is fluidized with 0.5m/s gas velocity, granularity is basically unchanged, and blowout mass loss is less than 0.5%.
Embodiment 2
The present embodiment selects the main component of ilmenite：TiO2：47.8%, FeO：37.81%, Fe2O3：3.66%, MgO：
6.28%, CaO：0.83%, SiO2：2.32%, Al2O3：1.23%；Its size distribution is between 60~200 mesh, average particle size
It is 194 μm；Specific preparation process is as follows：
A, by ilmenite in fluid bed 950 DEG C of oxidizing roasting 1.5h under air atmosphere, obtain the oxygen that oxygenation efficiency is 93%
Change mine；
B, by oxide ore in fluid bed 800 DEG C of reduction roasting 0.5h under coke-stove gas, obtain reduction rate be 91% also
Raw ore；
C, by reduced ore in fluid bed 950 DEG C of oxidizing roasting 0.3h under air atmosphere, it is 82% again to obtain oxygenation efficiency
Oxide ore；
D, mining 20 weight % hydrochloric acid will be reoxidized in the flask with strong mixing (rotating speed 500r/min), liquid-solid ratio
4：1 (L/kg), temperature are to leach 4h at 105 DEG C, are separated by solid-liquid separation, obtain leaching solid phase and leachate, 98% or more solid phase grain
Degree is distributed between 60~200 mesh, and average particle size is 191 μm；
E, will leach solid phase with 8 weight %NaOH in liquid-solid ratio 2：1 (L/kg), temperature be 50 DEG C at leach 0.5h, Gu
After liquid separation, it is washed with water and washs 2 times after washing 1 time with the leachate of step D, obtain synthetic rutile first product, synthetic rutile
First product 500 DEG C of calcining 1h in rotary kiln, obtain high-strength artificial rutile product.
High-strength artificial rutile product obtained by the present embodiment, 98% or more size distribution are average between 60~200 mesh
Granularity is 191 μm, and main component is：TiO2：96.23%, FeO：1.67%, MgO：0.58%, CaO：0.09%, SiO2：
0.94%, Al2O3：The rate of recovery of 0.40%, whole process Ti are 98.3%, and verification test shows the product in cold conditions gas-solid flow
Change in bed and uses N22h is fluidized with 0.5m/s gas velocity, granularity is basically unchanged, and blowout mass loss is less than 0.5%.
Comparative example 1 (does not reoxidize process)
The ilmenite of this comparative example selection example 1, specific preparation process are as follows：
A, by ilmenite in fluid bed 1000 DEG C of oxidizing roasting 1h under air atmosphere, obtain the oxidation that oxygenation efficiency is 95%
Mine；
B, by oxide ore in fluid bed 750 DEG C of reduction roasting 1h under coke-stove gas, obtain the reduction that reduction rate is 91%
Mine；
C, mining 20 weight % hydrochloric acid will be restored in the reactor with strong mixing (rotating speed 500r/min), liquid-solid ratio
4：1 (L/kg), temperature are to leach 4h at 105 DEG C, are separated by solid-liquid separation, and obtain leaching solid phase and leachate, and solid particle is averaged grain
Degree is only 26 μm, less than 10% between 60~200 mesh；
D, will leach solid phase with 8 weight %NaOH in liquid-solid ratio 2：1 (L/kg), temperature be 50 DEG C at leach 0.5h, Gu
After liquid separation, it is washed with water and washs 2 times after washing 1 time with the leachate of step C, obtain synthetic rutile first product, synthetic rutile
First product 500 DEG C of calcining 1h in rotary kiln, obtain synthetic rutile product.
Synthetic rutile product obtained by this comparative example, size distribution original particle size between 60~200 mesh less than 10%,
Average particle size is 22 μm, and main component is：TiO2：93.87%, FeO：2.19%, MgO：0.65%, CaO：0.10%, SiO2：
2.12%, Al2O3：0.63%, the rate of recovery of whole process Ti is 90%, and since its granularity is too small, does not meet boiling completely
Chlorination requirement, does not carry out fluidisation verification test.
Comparative example 2 (does not reoxidize process, salt Ore Leaching does not stir)
The ilmenite of this comparative example selection example 1, specific preparation process are as follows：
A, by ilmenite in fluid bed 1000 DEG C of oxidizing roasting 1h under air atmosphere, obtain the oxidation that oxygenation efficiency is 95%
Mine；
B, by oxide ore in fluid bed 750 DEG C of reduction roasting 1h under coke-stove gas, obtain the reduction that reduction rate is 91%
Mine；
C, mining 20 weight % hydrochloric acid will be restored in the reactor without stirring, liquid-solid ratio is 4：1 (L/kg), temperature are
4h is leached at 105 DEG C, is separated by solid-liquid separation, and obtains leaching solid phase and leachate, solid particle average particle size is 97 μm, 60~200
Particle is only 48% between mesh；
D, will leach solid phase with 8 weight %NaOH in liquid-solid ratio 2：1 (L/kg), temperature be 50 DEG C at leach 0.5h, Gu
After liquid separation, it is washed with water and washs 2 times after washing 1 time with the leaching waste liquid of step C, obtain synthetic rutile first product, artificial golden red
Stone first product 500 DEG C of calcining 1h in rotary kiln, obtain synthetic rutile product.
Synthetic rutile product obtained by this comparative example, size distribution original particle size are only 47% between 60~200 mesh, are put down
Equal granularity is 94 μm, and main component is：TiO2：93.87%, FeO：2.19%, MgO：0.65%, CaO：0.10%, SiO2：
2.12%, Al2O3：The rate of recovery of 0.63%, whole process Ti are 92%, and verification test shows that the product is gas-solid fluidized in cold conditions
N is used in bed22h is fluidized with 0.5m/s gas velocity, average particle size is reduced to 71 μm, and blowout mass loss reaches 31%.
Claims (9)
1. the method that ilmenite prepares high-strength artificial rutile, it is characterised in that：Include the following steps：
A, the oxidized roasting of ilmenite obtains the oxide ore of oxygenation efficiency >=80%；
B, oxide ore obtained by step A obtains the reduced ore of reduction rate >=80% in reducing atmosphere through reduction roasting；
C, the oxidized roasting of reduced ore obtained by step B, obtain oxygenation efficiency >=50% reoxidizes mine；
D, mining inorganic Ore Leaching is reoxidized obtained by step C, solid-liquor separation must leach solid phase；
E, solid phase is leached obtained by step D to be leached with inorganic alkali solution, through solid-liquor separation, washing, obtain synthetic rutile first product, first product
Through calcining, high-strength artificial rutile is obtained.
2. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step A,
At least meet it is following in one：
TiO containing 40~60 weight % in the ilmenite2With the SiO of 1~8 weight %2；
The size distribution of the ilmenite is 60~200 mesh.
3. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step A,
The temperature of the oxidizing roasting is 850~1050 DEG C；The time of the oxidizing roasting is 0.5~2h.
4. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step B,
The temperature of the reduction roasting is 700~800 DEG C；The time of the reduction roasting is 0.5~4h.
5. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step C,
The temperature of the oxidizing roasting is 850~1050 DEG C；The time of the oxidizing roasting is 0.2~0.5h.
6. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step D,
At least meet it is following in one：
The inorganic acid is hydrochloric acid or sulfuric acid；
A concentration of 15~25 weight % of the inorganic acid；
The inorganic acid and the volume mass ratio for reoxidizing mine are 3~4：1.
7. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step D,
At least meet it is following in one：
When inorganic Ore Leaching, control mixing speed is 200~500r/min；
The temperature of the leaching is 80~105 DEG C；
The time of the leaching is 2~6h.
8. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step E,
At least meet it is following in one：
The inorganic base is NaOH or KOH；
A concentration of 5~15 weight % of the inorganic alkali solution；
The inorganic alkali solution is 1~3 with the volume mass ratio for leaching solid phase：1.
9. the method that ilmenite according to claim 1 prepares high-strength artificial rutile, it is characterised in that：In step E,
At least meet it is following in one：
The temperature of the leaching is 30~80 DEG C；
The time of the leaching is 0.5~1h；
The temperature of the calcining is 300~700 DEG C；
The time of the calcining is 0.2~1h.
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| RU2687363C1 (en) * | 2018-11-06 | 2019-05-13 | Публичное Акционерное Общество "Корпорация Всмпо-Ависма" | Method of producing artificial rutile from ilmenite concentrates |
| CN113088683A (en) * | 2021-04-21 | 2021-07-09 | 重庆大学 | Method for preparing low-temperature titanium chloride slag by using low-grade titanium concentrate |
| CN113549345A (en) * | 2021-08-26 | 2021-10-26 | 苏州市宏丰钛业有限公司 | Preparation method and system of titanium dioxide for plastics |
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| CN113088683B (en) * | 2021-04-21 | 2022-11-04 | 重庆大学 | Method for preparing low-temperature titanium chloride slag by using low-grade titanium concentrate |
| CN113549345A (en) * | 2021-08-26 | 2021-10-26 | 苏州市宏丰钛业有限公司 | Preparation method and system of titanium dioxide for plastics |
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