CN117206068A - Recovery method of acidolysis waste residue of titanium dioxide by sulfuric acid method and application thereof - Google Patents
Recovery method of acidolysis waste residue of titanium dioxide by sulfuric acid method and application thereof Download PDFInfo
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- CN117206068A CN117206068A CN202311178409.8A CN202311178409A CN117206068A CN 117206068 A CN117206068 A CN 117206068A CN 202311178409 A CN202311178409 A CN 202311178409A CN 117206068 A CN117206068 A CN 117206068A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 193
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 238000000034 method Methods 0.000 title claims abstract description 139
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 88
- 239000002699 waste material Substances 0.000 title claims abstract description 73
- 238000011084 recovery Methods 0.000 title claims description 22
- 239000012141 concentrate Substances 0.000 claims abstract description 134
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 107
- 230000002000 scavenging effect Effects 0.000 claims abstract description 100
- 239000010936 titanium Substances 0.000 claims abstract description 100
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 99
- 230000005484 gravity Effects 0.000 claims abstract description 67
- 238000007885 magnetic separation Methods 0.000 claims abstract description 27
- 238000004064 recycling Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims description 35
- 239000007787 solid Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 4
- 235000010215 titanium dioxide Nutrition 0.000 description 73
- 239000012535 impurity Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 238000003825 pressing Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002516 radical scavenger Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000006148 magnetic separator Substances 0.000 description 6
- 239000002910 solid waste Substances 0.000 description 6
- 238000004537 pulping Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 241001417527 Pempheridae Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of sulfuric acid process titanium dioxide tailings treatment, in particular to a method for recycling sulfuric acid process titanium dioxide acidolysis waste residues and application thereof. The method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method comprises the following steps: carrying out wet magnetic separation and roughing on slurry containing acidolysis waste residues of titanium dioxide by a sulfuric acid method to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings; carrying out gravity scavenging on wet magnetic roughing tailings to obtain gravity scavenging concentrate and gravity scavenging tailings; the electric scavenging concentrate is obtained after the electric scavenging of the gravity scavenging tailings; mixing the electric scavenging concentrate with the wet magnetic roughing concentrate and the gravity scavenging concentrate to obtain a titanium concentrate roughing ore; and (3) carrying out electric concentration on the rough titanium concentrate ore to obtain titanium concentrate. The method can effectively recycle the titanium concentrate in the acidolysis waste residue of the titanium dioxide by the sulfuric acid method, the grade of the obtained titanium concentrate is more than 50%, and the titanium yield is more than 70%.
Description
Technical Field
The invention relates to the technical field of sulfuric acid process titanium dioxide tailings treatment, in particular to a method for recycling sulfuric acid process titanium dioxide acidolysis waste residues and application thereof.
Background
The traditional titanium white production process is mainly divided into a sulfuric acid process and a chlorination process, and is limited by production technology and titanium ore types, and most titanium white is produced by the sulfuric acid process at present. The sulfuric acid method has lower requirements on raw materials, so that a large amount of acidolysis tailings can be generated in the production process, and according to statistics, 0.5t acidolysis tailings can be generated per 1t of titanium white produced, and if the acidolysis tailings are piled, the resource waste can be caused, and the environment protection is not facilitated. How to effectively treat acidolysis tailings, recycle titanium resources, reduce solid waste discharge, improve the reutilization rate of resources, and have important practical significance for effective utilization of resources and environmental protection.
Sulfuric acid hydrolysis tailings are one of waste products generated in the sulfuric acid process titanium dioxide production process, and are generated through settlement and hot filtration of acidolysis titanium liquid. Because sulfuric acid can not finally remove TiO in the titanium concentrate in the acidolysis process 2 Fully react to form TiOSO 4 Or Ti (SO) 4 ) 2 The acidolysis rate was about 96%. Thus, part of the unreacted TiO is still carried in the acidolysis sludge 2 Finally, the sludge is discarded, and the loss of titanium is large.
Regarding the recycling of acidolysis tailings, early acidolysis tailings are added as solid waste into building materials such as cement and the like. In recent years, researches on acidolysis tailings titanium resource recovery technology mainly include methods such as an acid leaching method, an extraction method, a flotation method, a magnetic separation method, a gravity separation method and the like. However, the single magnetic separation method or the gravity separation method cannot fully recover the titanium in the waste residue, so that the overall titanium yield is low; meanwhile, the introduction of gangue components in the separation process causes the introduction of silicon, calcium and magnesium impurities, so that the grade of titanium is lower, and the gangue components can be only used as titanium middlings for blending.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method, which can effectively recycle titanium concentrate in acidolysis waste residues of titanium dioxide by the sulfuric acid method, and the obtained titanium concentrate has high grade.
The second purpose of the invention is to provide the application of the titanium concentrate obtained by the recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method in preparation of titanium dioxide and titanium sponge, thereby reducing solid waste discharge and improving the recycling rate of resources.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the invention provides a method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method, which comprises the following steps:
(a) Carrying out wet magnetic separation and roughing on slurry containing acidolysis waste residues of titanium dioxide by a sulfuric acid method to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings;
(b) Carrying out gravity scavenging on wet magnetic roughing tailings to obtain gravity scavenging concentrate and gravity scavenging tailings;
(c) The recleaning scavenging tailings are subjected to electric scavenging to obtain electric scavenging concentrate; mixing the electric scavenging concentrate with the wet magnetic roughing concentrate in the step (a) and the gravity scavenging concentrate in the step (b) to obtain a titanium concentrate roughing ore;
(d) And (3) carrying out electric separation and concentration on the rough titanium concentrate ore to obtain titanium concentrate.
The invention also provides application of the titanium concentrate obtained by the recovery method of acidolysis waste residues of titanium dioxide by the sulfuric acid method in preparation of titanium dioxide and titanium sponge.
Compared with the prior art, the invention has the beneficial effects that:
(1) The recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method can obtain high-grade titanium concentrate, thereby reducing solid waste discharge, improving the recycling rate of resources and reducing the production cost.
(2) The recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the invention has the advantages of simple process, mild condition and easiness in realizing batch production.
(3) According to the recovery method of acidolysis waste residues of titanium dioxide by the sulfuric acid method, provided by the invention, the titanium grade and the titanium yield are further improved by adopting specific parameters such as magnetic field intensity, stroke frequency, preheating temperature, voltage and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a process flow chart of the method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and detailed description, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative of the present invention only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In a first aspect, the invention provides a method for recovering acidolysis waste residues of titanium dioxide by a sulfuric acid method, in particular to a method for recovering titanium concentrate by acidolysis waste residues of titanium dioxide by a sulfuric acid method, which is shown in a process flow chart of the method for recovering acidolysis waste residues of titanium dioxide by the sulfuric acid method in fig. 1, and specifically comprises the following steps:
(a) And carrying out wet magnetic separation and roughing on the slurry containing the acidolysis waste residues of the titanium dioxide by the sulfuric acid method to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(b) And (c) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (a) to obtain gravity scavenging concentrate and gravity scavenging tailings.
(c) And (c) carrying out electric scavenging on the gravity scavenging tailings obtained in the step (b) to obtain electric scavenging concentrate.
And then mixing the electric scavenging concentrate with the wet magnetic roughing concentrate obtained in the step (a) and the gravity scavenging concentrate obtained in the step (b) to obtain the titanium concentrate roughing.
(d) And (c) carrying out electric concentration on the rough titanium concentrate ore obtained in the step (c) to obtain titanium concentrate.
The invention processes acidolysis waste residue of titanium dioxide by sulfuric acid method, which is acidolysis tailings generated in the process of producing titanium dioxide by sulfuric acid method, is generated by sedimentation and hot filtration of acidolysis titanium liquid, and contains TiO which does not react with sulfuric acid 2 。
According to the recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method, provided by the invention, titanium resources are recovered by adopting wet magnetic separation roughing, gravity separation scavenging, electric separation concentration and other means, so that high-grade titanium concentrate can be obtained, solid waste emission is reduced, and the recycling rate of the resources is improved.
Specifically, the method carries out magnetic separation, gravity separation and electric separation on acidolysis waste residues of titanium dioxide by a sulfuric acid method, so that titanium dioxide in the waste residues can be efficiently enriched to obtain high-grade titanium concentrate; meanwhile, according to the difference of gangue impurities, ilmenite magnetism, specific gravity and conductivity in the acidolysis waste residue of the titanium dioxide by a sulfuric acid method, the method obtains higher titanium yield through step separation of magnetic separation, reselection and electric separation, fully extracts titanium dioxide in the waste residue, and greatly meets the reduction and harmless treatment principles of waste.
The titanium element in the acidolysis waste residue of the titanium dioxide by the sulfuric acid method consists of an unreacted ilmenite phase and a rutile phase which is difficult to acidolysis, and the impurity phase mainly comprises silicon dioxide impurities which do not participate in acidolysis reaction and other impurities such as calcium, magnesium, aluminum and the like; in addition, as fine particles exist in acidolysis tailings after acidolysis reaction in the production process of titanium dioxide by a sulfuric acid method, dust emission can be effectively avoided by adopting a wet magnetic separation mode, and a good separation effect is ensured.
However, ilmenite cannot be completely recovered by one-time magnetic separation, and rutile which is difficult to acidolysis is not recovered; according to the invention, by adopting gravity separation, according to the principle that ilmenite and rutile have larger specific gravity, a small part of ilmenite which is not recovered by magnetic separation in the magnetic separation roughing tailings is separated from nonmagnetic rutile and impurities, so that gravity separation scavenging concentrate taking ilmenite and rutile as main bodies is obtained.
The rutile is difficult to be completely enriched into the concentrate through one-time gravity separation, and according to the principle that the rutile has conductivity and the impurities such as silicon dioxide do not have conductivity, the rutile in the gravity separation scavenging tailings is further separated, so that the electric scavenging concentrate taking the rutile as a main body is obtained.
Impurities are introduced into the inevitable re-enrichment process of the titanium concentrate coarse ore obtained by combining the magnetic separation coarse concentrate, the gravity separation scavenging concentrate and the electric separation scavenging concentrate, and according to the principle that ilmenite and rutile have conductivity and impurities such as silicon dioxide do not have conductivity, the impurities can be removed through electric separation, the titanium grade is improved, the added value is improved, and the downstream application range is improved.
In some specific embodiments, the titanium concentrate obtained by the method has a titanium grade of more than 50% and a titanium yield of more than 70%.
In addition, the recovery method of acidolysis waste residues of titanium dioxide by the sulfuric acid method provided by the invention has the advantages of simple process, mild conditions and easiness in realizing batch production.
In some specific embodiments, in step (a), the solid content of the slurry containing acidolysis waste residue of titanium dioxide in sulfuric acid process is 20% -35%, including but not limited to any one of the point values or any range value between the two of 20%, 23%, 25%, 28%, 30%, 32%, 35%.
In some specific embodiments, in step (a), the magnetic field strength of the wet magnetic separation rougher is 4000GS to 8000GS, including but not limited to any one of the point values or a range between any two of 4000GS, 5000GS, 6000GS, 7000GS, 8000GS.
According to the invention, by adopting wet magnetic separation with medium magnetic field strength, the ilmenite phase in the tailings can be effectively separated from other components, and the magnetic separation roughing concentrate taking ilmenite as a main component is obtained.
In some specific embodiments, in step (b), the reselection sweep is 15mm to 30mm in stroke, including but not limited to a point value of any one of 15mm, 18mm, 20mm, 23mm, 25mm, 28mm, 30mm, or a range of values therebetween.
In some specific embodiments, in the step (b), the washing frequency of the reselection and the scavenging is 200 times/min to 300 times/min, including but not limited to a point value of any one of 200 times/min, 220 times/min, 240 times/min, 250 times/min, 270 times/min, 290 times/min, 300 times/min or a range value between any two.
By adopting the gravity separation scavenging parameters, ilmenite and rutile are conveniently separated from impurities.
In some embodiments, in step (c), the apparatus used for the reselection and the scavenger comprises a shaker.
In some specific embodiments, in step (c), the gravity scavenger tail is dried and first preheated prior to the electric scavenger.
In some specific embodiments, the temperature of the first preheat is 120 ℃ to 150 ℃, including, but not limited to, a point value of any one of 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃ or a range value between any two.
In some specific embodiments, in step (c), the voltage of the electric sweeper is 14000V to 18000V, including but not limited to a point value of any one of 14000V, 15000V, 16000V, 17000V, 18000V, or a range value between any two.
The adoption of the first preheating temperature and the electric scavenging voltage is favorable for further separating rutile, and further improves the titanium yield.
In some specific embodiments, in step (c), the electric scavenger concentrate is produced by electric scavenger and the electric scavenger tailings are also produced, wherein the electric scavenger tailings are waste.
Titanium dioxide in the electric-separation scavenging tailings obtained through magnetic separation, reselection and electric separation is difficult to recover and is thrown away together with other impurities.
In some embodiments, in step (d), the titanium concentrate raw ore is dried and a second pre-heated.
In some specific embodiments, the second preheating temperature is 120 ℃ to 150 ℃, including but not limited to, a point value of any one of 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃ or a range value between any two.
In some specific embodiments, in the step (c), the wet magnetic roughing concentrate obtained in the step (a) and the gravity scavenging concentrate obtained in the step (b) are mixed, press-filtered and dried, and then mixed with the electric scavenging concentrate.
In some specific embodiments, in step (d), the selected voltage is 18000V to 22000V, including but not limited to any one of 18000V, 19000V, 20000V, 21000V, 22000V, or a range of values therebetween.
The adoption of the second preheating temperature and the electric selection concentration voltage is beneficial to further removing impurities so as to improve the grade of titanium.
In some specific embodiments, in the step (d), after the rough titanium concentrate is subjected to electric concentration, electric concentration concentrate and electric concentration tailings are obtained, wherein the electric concentration concentrate is the titanium concentrate. The electric separation tailings can be collected and mixed with the gravity separation tailings in the next flow to carry out electric separation scavenging.
Part of ilmenite and rutile enter the electric separation tailings in the electric separation and concentration process due to finer acidolysis tailings, and the electric separation tailings have higher titanium grade due to lower impurity content in the titanium concentrate coarse ore, so that the electric separation tailings can be returned to be mixed with the gravity separation tailings for separation again, and the recovery rate of the whole titanium dioxide can be further improved.
In some embodiments, in step (d), the TiO in the titanium concentrate 2 Mass fraction (i.e. grade of titanium concentrate)>50%, including but not limited to any one of, or a range of values between, point values of 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 60%, 62%, 65%, 67%, 70%.
In some specific embodiments, the recovery method of acidolysis waste residue of titanium dioxide by sulfuric acid method is used for recovering titanium concentrate, and the overall titanium yield is more than 70% and includes, but is not limited to, any one of point values or range values between any two of 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 82%, 85%.
Wherein, the overall titanium yield is the percentage of the mass of titanium dioxide in the recovered titanium concentrate to the mass of titanium dioxide in acidolysis waste residue of titanium dioxide by a sulfuric acid method.
In a second aspect, the invention also provides application of the titanium concentrate obtained by the method for recycling the acidolysis waste residues of titanium dioxide by the sulfuric acid method in preparation of titanium dioxide and titanium sponge.
The method enriches the acidolysis tailings of the titanium sulfate white into high-grade titanium concentrate, can be directly suitable for the production of titanium dioxide and titanium sponge, comprehensively recovers the downstream waste residues of the titanium white as an upstream raw material, has important significance for supplementing the raw material of the titanium dioxide, and reduces the cost.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In the acidolysis waste residues of the titanium dioxide by the sulfuric acid method, which are treated in the following examples, the mass fraction of titanium dioxide is 26.52wt.% (tailings of the same batch).
Example 1
The recycling method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment comprises the following steps:
(1) Mixing acidolysis waste residue of titanium dioxide by sulfuric acid method with water, and pulping to obtain slurry with solid content of 25%. And carrying out wet magnetic separation roughing on the slurry through a wet magnetic separator under the magnetic field strength of 6000GS to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(2) And (3) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (1) through a shaking table, wherein the stroke is 20mm, and the flushing frequency is 250 times/min, so as to obtain gravity scavenging concentrate and gravity scavenging tailings.
(3) And (3) carrying out filter pressing and drying on the gravity scavenging tailings obtained in the step (2), preheating the dried gravity scavenging tailings to 150 ℃ (namely, first preheating), and then carrying out electric scavenging, wherein the voltage is 16000V, so as to obtain electric scavenging concentrate.
And (3) mixing the wet magnetic roughing concentrate obtained in the step (1) and the gravity scavenging concentrate obtained in the step (2), then carrying out filter pressing and drying, and then mixing with the electric scavenging concentrate to obtain the titanium concentrate roughing.
(4) And (3) preheating the rough titanium concentrate ore obtained in the step (3) to 150 ℃ (namely, second preheating), and then carrying out electric separation and concentration, wherein the voltage is 20000V, so as to obtain the titanium concentrate.
Example 2
The recycling method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment comprises the following steps:
(1) Mixing acidolysis waste residue of titanium dioxide by sulfuric acid method with water, and pulping to obtain slurry with solid content of 30%. And carrying out wet magnetic separation roughing on the slurry through a wet magnetic separator under the magnetic field strength of 7000GS to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(2) And (3) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (1) through a shaking table, wherein the stroke is 30mm, and the stroke frequency is 280 times/min, so as to obtain gravity scavenging concentrate and gravity scavenging tailings.
(3) And (3) carrying out filter pressing and drying on the gravity scavenging tailings obtained in the step (2), preheating the dried gravity scavenging tailings to 140 ℃ (namely, first preheating), and then carrying out electric scavenging, wherein the voltage is 18000V, so as to obtain electric scavenging concentrate.
And (3) mixing the wet magnetic roughing concentrate obtained in the step (1) and the gravity scavenging concentrate obtained in the step (2), then carrying out filter pressing and drying, and then mixing with the electric scavenging concentrate to obtain the titanium concentrate roughing.
(4) And (3) preheating the rough titanium concentrate ore obtained in the step (3) to 140 ℃ (namely, second preheating), and then carrying out electric separation and concentration, wherein the voltage is 18000V, so as to obtain the titanium concentrate.
Example 3
The recycling method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment comprises the following steps:
(1) Mixing acidolysis waste residue of titanium dioxide by sulfuric acid method with water, and pulping to obtain slurry with solid content of 28%. And carrying out wet magnetic separation roughing on the slurry by a wet magnetic separator under the magnetic field strength of 8000GS to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(2) And (3) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (1) through a shaking table, wherein the stroke is 25mm, and the stroke frequency is 260 times/min, so as to obtain gravity scavenging concentrate and gravity scavenging tailings.
(3) And (3) carrying out filter pressing and drying on the gravity scavenging tailings obtained in the step (2), preheating the dried gravity scavenging tailings to 130 ℃ (namely, first preheating), and then carrying out electric scavenging, wherein the voltage is 17000V, so as to obtain electric scavenging concentrate.
And (3) mixing the wet magnetic roughing concentrate obtained in the step (1) and the gravity scavenging concentrate obtained in the step (2), then carrying out filter pressing and drying, and then mixing with the electric scavenging concentrate to obtain the titanium concentrate roughing.
(4) And (3) preheating the rough titanium concentrate ore obtained in the step (3) to 130 ℃ (namely, second preheating), and then carrying out electric concentration, wherein the voltage is 19000V, so as to obtain the titanium concentrate.
Example 4
The recycling method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment comprises the following steps:
(1) Mixing acidolysis waste residue of titanium dioxide by sulfuric acid method with water, and pulping to obtain slurry with solid content of 25%. And carrying out wet magnetic separation roughing on the slurry through a wet magnetic separator under the magnetic field strength of 5000GS to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(2) And (3) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (1) through a shaking table, wherein the stroke is 18mm, and the stroke frequency is 200 times/min, so as to obtain gravity scavenging concentrate and gravity scavenging tailings.
(3) And (3) carrying out filter pressing and drying on the gravity scavenging tailings obtained in the step (2), preheating the dried gravity scavenging tailings to 120 ℃ (namely, first preheating), and then carrying out electric scavenging, wherein the voltage is 16000V, so as to obtain electric scavenging concentrate.
And (3) mixing the wet magnetic roughing concentrate obtained in the step (1) and the gravity scavenging concentrate obtained in the step (2), then carrying out filter pressing and drying, and then mixing with the electric scavenging concentrate to obtain the titanium concentrate roughing.
(4) And (3) preheating the rough titanium concentrate ore obtained in the step (3) to 120 ℃ (namely, second preheating), and then carrying out electric separation and concentration, wherein the voltage is 21000V, so as to obtain the titanium concentrate.
Example 5
The recycling method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment comprises the following steps:
(1) Mixing acidolysis waste residue of titanium dioxide by sulfuric acid method with water, and pulping to obtain slurry with solid content of 20%. And carrying out wet magnetic separation roughing on the slurry through a wet magnetic separator under the magnetic field strength of 4000GS to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings.
(2) And (3) carrying out gravity scavenging on the wet magnetic roughing tailings obtained in the step (1) through a shaking table, wherein the stroke is 15mm, and the stroke frequency is 300 times/min, so as to obtain gravity scavenging concentrate and gravity scavenging tailings.
(3) And (3) carrying out filter pressing and drying on the gravity scavenging tailings obtained in the step (2), preheating the dried gravity scavenging tailings to 130 ℃ (namely, first preheating), and then carrying out electric scavenging, wherein the voltage is 14000V, so as to obtain electric scavenging concentrate.
And (3) mixing the wet magnetic roughing concentrate obtained in the step (1) and the gravity scavenging concentrate obtained in the step (2), then carrying out filter pressing and drying, and then mixing with the electric scavenging concentrate to obtain the titanium concentrate roughing.
(4) And (3) preheating the rough titanium concentrate ore obtained in the step (3) to 130 ℃ (namely, second preheating), and then carrying out electric concentration, wherein the voltage is 22000V, so as to obtain the titanium concentrate.
Example 6
The recovery method of acidolysis waste residues of titanium dioxide by sulfuric acid method provided in this example is basically the same as that of example 5, except that in step (1), the solid content of the slurry is replaced by 45%, and the magnetic field strength of wet magnetic separation roughing is replaced by 12000GS.
Example 7
The recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the embodiment is basically the same as that of the embodiment 5, and the difference is that in the step (2), the stroke of the reselection and the scavenging is replaced by 5mm, and the stroke frequency is replaced by 100 times/min.
Example 8
The recovery method of acidolysis waste residues of titanium dioxide by sulfuric acid method provided by the embodiment is basically the same as that of the embodiment 5, and the difference is that in the step (4), the voltage for electric selection and selection is replaced by 10000V.
Comparative example 1
The recovery method of acidolysis waste residues of titanium dioxide by a sulfuric acid method provided by the comparative example is basically the same as that of the example 5, and is different in that dry magnetic separation roughing is adopted in the step (1), and the specific method is as follows: and carrying out dry magnetic separation on the sulfuric acid process titanium dioxide acidolysis waste residues by a permanent magnet dry magnetic separator under the magnetic field strength of 6000GS to obtain dry magnetic roughing concentrate and dry magnetic roughing tailings.
And the wet magnetic roughing tailings in the step (2) of example 5 are replaced with the dry magnetic roughing tailings obtained in the comparative example, and the wet magnetic roughing concentrate in the step (3) of example 5 is replaced with the dry magnetic roughing concentrate obtained in the comparative example.
Comparative example 2
The recovery method of acidolysis waste residues of titanium dioxide by the sulfuric acid method provided by the comparative example is basically the same as that of the embodiment 5, and the difference is that the wet magnetic roughing tailings are directly subjected to electric scavenging instead of the gravity scavenging in the step (2).
Comparative example 3
The recovery method of acidolysis waste residue of titanium dioxide by sulfuric acid method provided by the comparative example is basically the same as that of the embodiment 5, and the difference is that in the step (3), the electric scavenging is not performed, but the gravity scavenging tailings are directly mixed with wet magnetic roughing concentrate and gravity scavenging concentrate to obtain the titanium concentrate roughing ore.
Comparative example 4
The method for recycling acidolysis waste residues of titanium dioxide by the sulfuric acid method provided by the comparative example is basically the same as that of the example 5, except that the electric selection is not performed in the step (3).
Experimental example
The grade and overall titanium yield of the titanium concentrates obtained in each example and each comparative example were examined, and the results are shown in Table 1.
Wherein the grade of the titanium concentrate refers to the mass fraction of titanium dioxide in the titanium concentrate.
The overall titanium yield is the percentage of the mass of titanium dioxide in the recovered titanium concentrate to the mass of titanium dioxide in acidolysis waste residue of titanium dioxide by a sulfuric acid method.
TABLE 1 grade and overall titanium yield results for each titanium concentrate
Referring to Table 1, it is understood that each of the parameters in the recovery process has a certain influence on the titanium grade or the titanium yield by comparing the titanium grade and the titanium yield of example 5 and examples 6 to 8.
The titanium grade and titanium yield of example 5 were slightly higher than those of examples 6-8, demonstrating that the use of the parameters of magnetic field strength, stroke frequency, etc. provided by the invention can further increase the titanium grade and titanium yield.
As can be seen from a comparison of the data of example 5 and comparative examples 1-4, each step has a significant impact on titanium grade and titanium yield. This shows that the recovery method of acidolysis waste residue of titanium dioxide by sulfuric acid method can obtain high grade titanium concentrate with high titanium yield.
Therefore, the recovery method of acidolysis waste residues of titanium dioxide by the sulfuric acid method can obtain high-grade titanium concentrate, and the titanium concentrate can be directly used for producing titanium dioxide and titanium sponge, so that the solid waste emission is reduced, the resource utilization rate is improved, and the production cost of titanium dioxide and titanium sponge is reduced.
While the invention has been illustrated and described with reference to specific embodiments, it is to be understood that the above embodiments are merely illustrative of the technical aspects of the invention and not restrictive thereof; those of ordinary skill in the art will appreciate that: modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some or all of the technical features thereof, without departing from the spirit and scope of the present invention; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions; it is therefore intended to cover in the appended claims all such alternatives and modifications as fall within the scope of the invention.
Claims (10)
1. The method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method is characterized by comprising the following steps of:
(a) Carrying out wet magnetic separation and roughing on slurry containing acidolysis waste residues of titanium dioxide by a sulfuric acid method to obtain wet magnetic roughing concentrate and wet magnetic roughing tailings;
(b) Carrying out gravity scavenging on wet magnetic roughing tailings to obtain gravity scavenging concentrate and gravity scavenging tailings;
(c) The recleaning scavenging tailings are subjected to electric scavenging to obtain electric scavenging concentrate; mixing the electric scavenging concentrate with the wet magnetic roughing concentrate in the step (a) and the gravity scavenging concentrate in the step (b) to obtain a titanium concentrate roughing ore;
(d) And (3) carrying out electric separation and concentration on the rough titanium concentrate ore to obtain titanium concentrate.
2. The method for recycling acidolysis waste residues of titanium dioxide by sulfuric acid process according to claim 1, wherein in the step (a), the solid content of the slurry containing acidolysis waste residues of titanium dioxide by sulfuric acid process is 20% -35%.
3. The method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method according to claim 1, wherein in the step (a), the magnetic field strength of the wet magnetic separation roughing is 4000-8000 GS.
4. The method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method according to claim 1, wherein in the step (b), the stroke of the reselection and the scavenging is 15-30 mm, and the stroke frequency is 200-300 times/min.
5. The method for recycling acidolysis waste residues of titanium dioxide by sulfuric acid method according to claim 1, wherein in the step (c), before the electric scavenging, the scavenging tailings are dried and preheated for the first time;
preferably, the temperature of the first preheating is 120 ℃ to 150 ℃.
6. The method for recycling acidolysis waste residues of titanium dioxide by a sulfuric acid method according to claim 1, wherein in the step (c), the voltage of electric separation and scavenging is 14000-18000V.
7. The method for recycling acidolysis waste residues of titanium dioxide by sulfuric acid method according to claim 1, wherein in the step (d), the rough ore of the titanium concentrate is dried and preheated for the second time;
preferably, the temperature of the second preheating is 120 ℃ to 150 ℃.
8. The method for recycling acidolysis waste residues of titanium dioxide by sulfuric acid method according to claim 1, wherein in the step (d), the voltage for electric selection is 18000V-22000V.
9. The recycling method of acidolysis waste residues of titanium dioxide by sulfuric acid method according to claim 1The method is characterized in that in the step (d), tiO in the titanium concentrate 2 Mass fraction of (2)>50％。
10. The use of the titanium concentrate obtained by the recovery method of acidolysis waste residues of titanium dioxide by sulfuric acid method according to any one of claims 1 to 9 in the preparation of titanium dioxide and titanium sponge.
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