CN102732727A - Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag - Google Patents
Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag Download PDFInfo
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- CN102732727A CN102732727A CN201210160961XA CN201210160961A CN102732727A CN 102732727 A CN102732727 A CN 102732727A CN 201210160961X A CN201210160961X A CN 201210160961XA CN 201210160961 A CN201210160961 A CN 201210160961A CN 102732727 A CN102732727 A CN 102732727A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 194
- 239000002893 slag Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 61
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract 32
- -1 vanadium-sodium-aluminum-silicon Chemical compound 0.000 title abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 83
- 238000000605 extraction Methods 0.000 claims abstract description 45
- 238000002425 crystallisation Methods 0.000 claims abstract description 40
- 230000008025 crystallization Effects 0.000 claims abstract description 40
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000002386 leaching Methods 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 65
- 239000004411 aluminium Substances 0.000 claims description 64
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 64
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical compound [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 47
- 239000011734 sodium Substances 0.000 claims description 41
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 39
- 229910052708 sodium Inorganic materials 0.000 claims description 39
- 239000012670 alkaline solution Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 15
- 238000005516 engineering process Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000049 pigment Substances 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 239000012452 mother liquor Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 11
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000012266 salt solution Substances 0.000 abstract 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 abstract 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 abstract 2
- 238000007865 diluting Methods 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000011268 mixed slurry Substances 0.000 abstract 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 162
- 238000003756 stirring Methods 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- WNQQFQRHFNVNSP-UHFFFAOYSA-N [Ca].[Fe] Chemical compound [Ca].[Fe] WNQQFQRHFNVNSP-UHFFFAOYSA-N 0.000 description 1
- JCCZVLHHCNQSNM-UHFFFAOYSA-N [Na][Si] Chemical compound [Na][Si] JCCZVLHHCNQSNM-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 239000011504 laterite Substances 0.000 description 1
- 229910001710 laterite Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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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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- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention discloses a method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag. The method comprises: mixing high vanadium-sodium-aluminum-silicon slag and a sodium hydroxide solution, carrying out a leaching reaction, and diluting the resulting slurry after completing the reaction to obtain a mixed slurry; carrying out thermal insulation filtering to obtain leached residue and a vanadium-containing alkaline sodium salt solution; and carrying out sodium vanadate crystallization on the vanadium-containing alkaline sodium salt solution to obtain sodium vanadate. The method of the present invention has the following advantages that: the reaction temperature is low; the dissolution rate is high; the high vanadium-sodium-aluminum-silicon slag treatment process can be performed under the wet condition; high temperature calcination is not required, and the method can be performed at the low temperature under the normal pressure; the reaction time can be shortened; the operation is easy; the process is simple and has good security; and the efficient vanadium extraction is achieved. With the method, problems of high reaction temperature, low vanadium recovery rate, large amount of wastewater and waste residue discharging, and the like of the traditional process for extracting vanadium from high vanadium-sodium-aluminum-silicon slag are fundamentally solved, and clean use of vanadium is achieved.
Description
Technical field
The present invention relates to a kind of treatment process of waste residue, especially a kind of method of from high vanadium sodium aluminium white residue, extracting vanadium.
Background technology
" high vanadium sodium aluminium white residue " is the solid waste that is produced when containing vanadium leachate with the dephosphorization of aluminium salt silica removal in the conventional vanadium slag sodium roasting vanadium-extracting technology, and its staple is: Na=6%, Al=8%, Si=12%, V=10%.High vanadium sodium aluminium white residue must cause the waste of resource and the detrimentally affect of environment like stacking or landfill.Handle the sodium white residue at present and mainly contain following dual mode: 1, the applied chemistry method is extracted sodium, the aluminium in the sodium white residue: Chinese patent publication number CN101054629A discloses a kind of method of method of treating sodium-silicon slag by chlorination; This technology adds reductive agent in the sodium white residue; Join continuously and carry out chlorination in the boiling chloridizing furnace; Realize one section selective chlorination of sodium element in the sodium white residue,, realize that valuable element separates through steps such as washing, roasting, condensation separation.One Chinese patent application publication number CN1597525A discloses the desiliconization slag treatment process in a kind of aluminum oxide production process; Sodium white residue and the alkali lye of this technology after with solid-liquid separation, milk of lime are heated to 120～200 ℃ of insulation stripping 45-150min mixing the back that stirs in the stripping jar, the solid-liquid separation dissolution fluid is delivered to laterite washing system in the alumina producing flow process.One Chinese patent application publication number CN101343076A discloses a kind of method with preparing micro-mist hydroted alumina with sodium-silica residue, handles the sodium white residue with the vitriol oil and gets acid sludge, with the stripping of acid sludge water, obtains alum liquor and silica gel then, produces fine aluminum hydroxide powder then.2, be that starting raw material prepares molecular sieve with the sodium white residue: Chinese patent publication number CN1562748A discloses the method for a kind of sodium white residue production washing with the 4A zeolite; This method makes washing through operations such as batching, sintering, stripping, crystallization and uses the 4A zeolite product after the sodium white residue is purified pre-treatment.Chinese patent publication number CN101139099A has introduced the another kind of technology of utilizing the sodium white residue to produce the 4A zeolite; This technology utilizes acid regulator solution that the sodium white residue is leached reaction earlier; Filter residue joins in the alkaline regulator solution and reacts; Add and to lead brilliant auxiliary agent, synthesize, crystallization, oven dry obtain the 4A zeolite product.
The treatment process of above-mentioned sodium white residue is primarily aimed at the sodium white residue of aluminum oxide industry by-product; And the sodium white residue of the more above-mentioned aluminum oxide industry by-product of high vanadium sodium aluminium white residue that vanadium products factory vanadium liquid purification silica removal obtains has following difference: 1, the vanadiumcontent in the high vanadium sodium aluminium white residue is higher, contains elemental vanadium and is about 10%; 2, the calcium iron level in the high vanadium sodium aluminium white residue is higher relatively.Therefore.As handle high vanadium sodium aluminium white residue as stated above, except that the waste that causes vanadium, increasing of foreign matter content can cause adverse influence to the separation of each element in the leach liquor and the quality of molecular sieve.At present, the high vanadium sodium aluminium white residue of vanadium products factory mainly is to reclaim vanadium with washing or acidleach, but exists the recovery of vanadium low, and acid consumption is big, follow-up process for extracting vanadium has also been caused the problem of very big difficulty; And residual vanadium is higher in the gained tailings, can not recycling.
Summary of the invention
The technical problem that the present invention will solve provides the high method of from high vanadium sodium aluminium white residue, extracting vanadium of a kind of vanadium recovery.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: high vanadium sodium aluminium white residue is mixed with sodium hydroxide solution to change soak reaction, with the reaction paste dilution, obtain diluted slurry after reaction finishes; Then diluted slurry is incubated filtration, obtains leached mud and the sodium salt alkaline solution that contains vanadium, the said sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization, obtains vanadic acid sodium.
The present invention further adopts following process step: (1) batching: NaOH and high vanadium sodium aluminium white residue is even by weight the mixed of 0.25～2:1;
(2) commentaries on classics is soaked: in blended NaOH and high vanadium sodium aluminium white residue, add entry by solid-liquid weight ratio 1:1～4, change at 50～200 ℃ of following normal pressures then and soak 0.5～2h, obtain reaction paste;
(3) dilute filtration: water or NaOH solution are diluted to diluted slurry with reaction paste, and solid-liquid separation obtains leached mud and the sodium salt alkaline solution that contains vanadium then;
(4) crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization, obtains vanadic acid sodium.
The massfraction of NaOH solution is 1～15% in the step according to the invention (3).
Solid-liquid separation in the step according to the invention (3) is at 70～90 ℃ diluted slurry to be incubated filtration.
The leached mud that step according to the invention (3) obtains obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue after with water washing; The tailings in vanadium extraction of described high vanadium sodium aluminium white residue with carry out calcination process after the tailings in vanadium extraction of conventional vanadium slag mixes.Described vanadium slag is to obtain conventional vanadium slag in the steelmaking process, be vanadium-bearing hot metal is obtained through oxidation blowing in the vanadium extraction process or contain the vanadium iron concentrate through the resulting general designation that contains the bits of vanadium oxide of wet method vanadium extraction.
Described calcination process is: (1) batch mixing: the tailings in vanadium extraction of high vanadium sodium aluminium white residue is mixed by weight 1:5～1:100 with the tailings in vanadium extraction of vanadium slag, obtain mixing slag;
(2) roasting: mix slag at 700～900 ℃ of roasting 1～10h, cooling obtains fired slags;
(3) solid-liquid separation: the fired slags water logging is filtered, and obtains containing vanadium clear liquid and finishing slag; The described vanadium clear liquid that contains can be used for Leaching of Vanadium from Vanadium slag technology as mother liquor; Described finishing slag can be used as black porcelain and prepares pigment or solar panels heat-absorbing paint.
The sodium salt alkaline solution that contains vanadium in the step according to the invention (4) carries out the vanadic acid sodium crystallization under 0～40 ℃.
Liquid is used for the water described in the alternative steps (2) after the crystallization that step according to the invention (4) vanadic acid sodium crystallization obtains.
Adopt the beneficial effect that technique scheme produced to be: temperature of reaction of the present invention is low; The vanadium solubility rate is high, and high vanadium sodium aluminium white residue technology can be carried out under the wet method condition, does not need high-temperature roasting; Low-temperature atmosphere-pressure just can carry out down; Shorten the reaction times, easy handling and security are good, realize the high efficiency extraction of vanadium.In addition, in leaching process, the liquid phase of generation is returned and is leached the operation recycle, effectively reduces the generation and the output of waste water; The tailings that produces contains Na and is about 12%, is used for the baking mixed vanadium extraction of Leaching of Vanadium from Vanadium slag tailings, compares with traditional technology, and the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings has improved more than 10%; Last tailings can be used as that black porcelain prepares pigment and solar panels coating is sold outward, no waste generation, environmental friendliness.It is low that present method has overcome tradition (high vanadium sodium aluminium white residue) process for extracting vanadium vanadium recovery, and problems such as waste water and dregs discharging have realized that the cleaning of vanadium is recycled.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Embodiment 1: shown in Figure 1, this method of from high vanadium sodium aluminium white residue, extracting vanadium adopts following process step.
1, batching: NaOH and high vanadium sodium aluminium white residue stir by weight the mixed that is 1:1.
2, leach: blended NaOH and high vanadium sodium aluminium white residue are put in the reactor drum,, add entry, change at 110 ℃ of following normal pressures and soak 2.0h (liquid-phase oxidation among Fig. 1, leaching), obtain reaction paste by liquid-solid ratio 1:2.
3, dilute filtration: with 500mL water reaction paste is diluted to diluted slurry, under 80 ℃, diluted slurry is incubated filtration, obtain leached mud and the sodium salt alkaline solution (containing among Fig. 1 vanadium solution) that contains vanadium; The basicity that contains the sodium salt alkaline solution of vanadium is 48g/L.
4, washing: leached mud obtains the tailings in vanadium extraction (vanadium mud tailings in vanadium extraction among Fig. 1) of high vanadium sodium aluminium white residue with 80 ℃ water washing; Containing vanadium in this tailings is 0.35wt% (in vanadium), and the leaching yield of gained vanadium is 97.06%.
5, crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization under 40 ℃, liquid returns step 2 after the crystallization, replaces water wherein next time; The vanadic acid sodium crystallization can get in the purification vanadium liquid of Leaching of Vanadium from Vanadium slag technology carries out the ammonium precipitation.
6, tailings is handled:
(1) batch mixing: the tailings in vanadium extraction of high vanadium sodium aluminium white residue and the tailings in vanadium extraction of vanadium slag (the secondary slag among Fig. 1) by weight 1:10, are dropped in the stirrer and stir 10min, obtain mixing slag.
(2) roasting: mix slag at 800 ℃ of following roasting 4h, after the taking-up, naturally cool to room temperature, obtain fired slags.
(3) leach:, fired slags is mixed 90 ℃ of agitation leach 1h with gauge water by solid-to-liquid ratio 1:5.
(4) solid-liquid separation: leach mixed solution and filter, obtain containing vanadium clear liquid and finishing slag with the belt filter; Contain the vanadium clear liquid and incorporate the vanadium extraction flow process of vanadium slag as mother liquor into; Finishing slag can be used as black porcelain and prepares pigment or the sale of solar panels heat-absorbing paint.
With the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag baking mixed after, the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings is 58.2%.
Embodiment 2: this method of from high vanadium sodium aluminium white residue, extracting vanadium adopts following process step.
1, batching: NaOH (containing the NaOH in the liquid after the crystallization of returning) and high vanadium sodium aluminium white residue stir by weight for the mixed of 2:1.
2, leach: NaOH and high vanadium sodium aluminium white residue are put in the reactor drum,, soak 1.5h, obtain reaction paste 130 ℃ of following normal pressures commentaries on classics by liquid after the liquid-solid ratio 1:3 adding crystallization.
3, dilute filtration: using the 500mL massfraction is that 5% NaOH solution dilutes reaction paste, under 85 ℃, diluted slurry is incubated filtration, obtains leached mud and the sodium salt alkaline solution that contains vanadium; The basicity that contains the sodium salt alkaline solution of vanadium is 105g/L.
4, washing: leached mud obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue with 90 ℃ water washing; Containing vanadium in this tailings is 0.41wt% (in vanadium), and the leaching yield of gained vanadium is 96.58%.
5, crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization under 30 ℃, liquid returns step 2 after the crystallization, replaces water wherein next time; The vanadic acid sodium crystallization can be carried out the ammonium precipitation.
6, tailings is handled:
(1) batch mixing: the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag by weight 1:20, is dropped in the stirrer and stirs 10min, obtain mixing slag.
(2) roasting: mix slag at 750 ℃ of following roasting 10h, after the taking-up, naturally cool to room temperature, obtain fired slags.
(3) leach:, fired slags is mixed 100 ℃ of agitation leach 2h with gauge water by solid-to-liquid ratio 1:1.
(4) solid-liquid separation: leach mixed solution and filter, obtain containing vanadium clear liquid and finishing slag with the belt filter; Contain the vanadium clear liquid and incorporate the vanadium extraction flow process of vanadium slag as mother liquor into; Finishing slag can be used as black porcelain and prepares pigment or the sale of solar panels heat-absorbing paint.
With the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag baking mixed after, the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings is 56.6%.
Embodiment 3: this method of from high vanadium sodium aluminium white residue, extracting vanadium adopts following process step.
1, batching: NaOH (containing the NaOH in the liquid after the crystallization of returning) and high vanadium sodium aluminium white residue stir by weight for the mixed of 0.25:1.
2, leach: NaOH and high vanadium sodium aluminium white residue are put in the reactor drum,, soak 0.5h, obtain reaction paste 200 ℃ of following normal pressures commentaries on classics by liquid after the liquid-solid ratio 1:1 adding crystallization.
3, dilute filtration: using the 1000mL massfraction is that 1% NaOH solution dilutes reaction paste, under 90 ℃, diluted slurry is incubated filtration, obtains leached mud and the sodium salt alkaline solution that contains vanadium; The basicity that contains the sodium salt alkaline solution of vanadium is 22g/L.
4, washing: leached mud obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue with 70 ℃ water washing; Containing vanadium in this tailings is 0.51wt% (in vanadium), and the leaching yield of gained vanadium is 95.62%.
5, crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization under 25 ℃; The vanadic acid sodium crystallization can be carried out the ammonium precipitation.
6, tailings is handled:
(1) batch mixing: the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag by weight 3:20, is dropped in the stirrer and stirs 10min, obtain mixing slag.
(2) roasting: mix slag at 850 ℃ of following roasting 2h, after the taking-up, naturally cool to room temperature, obtain fired slags.
(3) leach:, fired slags is mixed 95 ℃ of agitation leach 5h with gauge water by solid-to-liquid ratio 1:3.
(4) solid-liquid separation: leach mixed solution and filter, obtain containing vanadium clear liquid and finishing slag with the belt filter.
With the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag baking mixed after, the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings is 59.1%.
Embodiment 4: this method of from high vanadium sodium aluminium white residue, extracting vanadium adopts following process step.
1, batching: NaOH (containing the NaOH in the liquid after the crystallization of returning) and high vanadium sodium aluminium white residue stir by weight for the mixed of 1.5:1.
2, leach: NaOH and high vanadium sodium aluminium white residue are put in the reactor drum,, soak 1.0h, obtain reaction paste 50 ℃ of following normal pressures commentaries on classics by liquid after the liquid-solid ratio 1:4 adding crystallization.
3, dilute filtration: using the 100mL massfraction is that 15% NaOH solution dilutes reaction paste, under 70 ℃, diluted slurry is incubated filtration, obtains leached mud and the sodium salt alkaline solution that contains vanadium; The basicity that contains the sodium salt alkaline solution of vanadium is 67g/L.
4, washing: leached mud obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue with 90 ℃ water washing; Containing vanadium in this tailings is 0.47wt% (in vanadium), and the leaching yield of gained vanadium is 96.81%.
5, crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization under 0 ℃, liquid returns step 2 after the crystallization, replaces water wherein next time; The vanadic acid sodium crystallization can be carried out the ammonium precipitation.
6, tailings is handled:
(1) batch mixing: the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag by weight 1:5, is dropped in the stirrer and stirs 5min, obtain mixing slag.
(2) roasting: mix slag at 900 ℃ of following roasting 1h, after the taking-up, naturally cool to room temperature, obtain fired slags.
(3) leach:, fired slags is mixed 50 ℃ of agitation leach 4h with gauge water by solid-to-liquid ratio 1:8.
(4) solid-liquid separation: leach mixed solution and filter, obtain containing vanadium clear liquid and finishing slag with the belt filter; Contain the vanadium clear liquid and incorporate the vanadium extraction flow process of vanadium slag as mother liquor into; Finishing slag can be used as black porcelain and prepares pigment or the sale of solar panels heat-absorbing paint.
With the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag baking mixed after, the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings is 57.8%.
Embodiment 5: this method of from high vanadium sodium aluminium white residue, extracting vanadium adopts following process step.
1, batching: NaOH and high vanadium sodium aluminium white residue stir by weight the mixed that is 0.75:1.
2, leach: NaOH and high vanadium sodium aluminium white residue are put in the reactor drum, and 1:2.5 adds entry by liquid-solid ratio, changes at 150 ℃ of following normal pressures and soaks 1.5h, obtains reaction paste.
3, dilute filtration: with 800mL water reaction paste is diluted, under 75 ℃, diluted slurry is incubated filtration, obtain leached mud and the sodium salt alkaline solution that contains vanadium; The basicity that contains the sodium salt alkaline solution of vanadium is 71g/L.
4, washing: leached mud obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue with 75 ℃ water washing; Containing vanadium in this tailings is 0.43wt% (in vanadium), and the leaching yield of gained vanadium is 95.98%.
5, crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization under 10 ℃, liquid returns step 2 after the crystallization, replaces water wherein next time; The vanadic acid sodium crystallization can be carried out the ammonium precipitation.
6, tailings is handled:
(1) batch mixing: the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag by weight 1:10, is dropped in the stirrer and stirs 20min, obtain mixing slag.
(2) roasting: mix slag at 700 ℃ of following roasting 8h, after the taking-up, naturally cool to room temperature, obtain fired slags.
(3) leach:, fired slags is mixed 80 ℃ of agitation leach 0.5h with gauge water by solid-to-liquid ratio 1:10.
(4) solid-liquid separation: leach mixed solution and filter, obtain containing vanadium clear liquid and finishing slag with the belt filter; Contain the vanadium clear liquid and incorporate the vanadium extraction flow process of vanadium slag as mother liquor into; Finishing slag can be used as black porcelain and prepares pigment or the sale of solar panels heat-absorbing paint.
With the tailings in vanadium extraction of the tailings in vanadium extraction of high vanadium sodium aluminium white residue and vanadium slag baking mixed after, the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings is 58.4%.
Shown in Figure 1; This extracts sinter process and present method combination of the method for vanadium with conventional Leaching of Vanadium from Vanadium slag technology, Leaching of Vanadium from Vanadium slag tailings (secondary slag) from high vanadium sodium aluminium white residue; Can improve the vanadium recovery of Leaching of Vanadium from Vanadium slag tailings; Product in the above-mentioned technology all can be fully utilized effectively, thereby save resource effectively, reduce discharging wastes, have the characteristics of energy-conserving and environment-protective.
Claims (8)
1. a method of from high vanadium sodium aluminium white residue, extracting vanadium is characterized in that: high vanadium sodium aluminium white residue is mixed with sodium hydroxide solution to change soak reaction, with the reaction paste dilution, obtain diluted slurry after reaction finishes; Then diluted slurry is incubated filtration, obtains leached mud and the sodium salt alkaline solution that contains vanadium, the said sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization, obtains vanadic acid sodium.
2. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 1 is characterized in that this method adopts following process step: (1) batching: NaOH and high vanadium sodium aluminium white residue is even by weight the mixed of 0.25～2:1;
(2) commentaries on classics is soaked: in blended NaOH and high vanadium sodium aluminium white residue, add entry by solid-liquid weight ratio 1:1～4, change at 50～200 ℃ of following normal pressures then and soak 0.5～2h, obtain reaction paste;
(3) dilute filtration: water or NaOH solution are diluted to diluted slurry with reaction paste, and solid-liquid separation obtains leached mud and the sodium salt alkaline solution that contains vanadium then;
(4) crystallization: the sodium salt alkaline solution that contains vanadium carries out the vanadic acid sodium crystallization, obtains vanadic acid sodium.
3. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 2 is characterized in that: the massfraction of NaOH solution is 1～15% in the said step (3).
4. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 2, it is characterized in that: the solid-liquid separation in the said step (3) is at 70～90 ℃ diluted slurry to be incubated filtration.
5. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 2 is characterized in that: the leached mud that said step (3) obtains obtains the tailings in vanadium extraction of high vanadium sodium aluminium white residue after with water washing; The tailings in vanadium extraction of described high vanadium sodium aluminium white residue with carry out calcination process after the tailings in vanadium extraction of conventional vanadium slag mixes.
6. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 5; It is characterized in that; Described calcination process is: (1) batch mixing: the tailings in vanadium extraction of high vanadium sodium aluminium white residue is mixed by weight 1:5～1:100 with the tailings in vanadium extraction of vanadium slag, obtain mixing slag;
(2) roasting: mix slag at 700～900 ℃ of roasting 1～10h, cooling obtains fired slags;
(3) solid-liquid separation: the fired slags water logging is filtered, and obtains containing vanadium clear liquid and finishing slag; The described vanadium clear liquid that contains can be used for Leaching of Vanadium from Vanadium slag technology as mother liquor; Described finishing slag can be used as black porcelain and prepares pigment or solar panels heat-absorbing paint.
7. the method for from high vanadium sodium aluminium white residue, extracting vanadium according to claim 2, it is characterized in that: the sodium salt alkaline solution that contains vanadium in the said step (4) carries out the vanadic acid sodium crystallization under 0～40 ℃.
8. from high vanadium sodium aluminium white residue, extract the method for vanadium according to described any one of claim 2-7, it is characterized in that: liquid is used for the water described in the alternative steps (2) after the crystallization that said step (4) vanadic acid sodium crystallization obtains.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291354A (en) * | 2013-07-20 | 2015-01-21 | 东北大学 | Method for preparation of zeolite 4A and vanadium-titanium catalyst from vanadium slag |
| CN104649320A (en) * | 2013-11-20 | 2015-05-27 | 中国科学院过程工程研究所 | Method of preparing vanadate of alkali metal from residue of aluminum powder vanadium removal of crude titanium tetrachloride |
| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
| US11247270B2 (en) | 2019-01-31 | 2022-02-15 | Na Wang | Method for preparing vanadium and vanadium alloy powder from vanadium-containing materials through shortened process |
| CN114291879A (en) * | 2021-11-23 | 2022-04-08 | 攀钢集团研究院有限公司 | Preparation method of aluminum silicate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102094123A (en) * | 2011-01-14 | 2011-06-15 | 河北钢铁股份有限公司承德分公司 | Method for extracting vanadium from vanadium-containing steel slag by using highly-alkaline sodium hydroxide medium |
| CN102127656A (en) * | 2010-01-13 | 2011-07-20 | 中国科学院过程工程研究所 | Method for decomposing vanadium slag by liquid phase oxidation |
| CN102127654A (en) * | 2010-01-13 | 2011-07-20 | 中国科学院过程工程研究所 | Method for decomposing chromium-containing vanadium slag by using sodium hydroxide molten salt |
| CN102251119A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院过程工程研究所 | Method for recycling vanadium extraction tailings |
-
2012
- 2012-05-23 CN CN201210160961.XA patent/CN102732727B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127656A (en) * | 2010-01-13 | 2011-07-20 | 中国科学院过程工程研究所 | Method for decomposing vanadium slag by liquid phase oxidation |
| CN102127654A (en) * | 2010-01-13 | 2011-07-20 | 中国科学院过程工程研究所 | Method for decomposing chromium-containing vanadium slag by using sodium hydroxide molten salt |
| CN102094123A (en) * | 2011-01-14 | 2011-06-15 | 河北钢铁股份有限公司承德分公司 | Method for extracting vanadium from vanadium-containing steel slag by using highly-alkaline sodium hydroxide medium |
| CN102251119A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院过程工程研究所 | Method for recycling vanadium extraction tailings |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291354A (en) * | 2013-07-20 | 2015-01-21 | 东北大学 | Method for preparation of zeolite 4A and vanadium-titanium catalyst from vanadium slag |
| CN104649320A (en) * | 2013-11-20 | 2015-05-27 | 中国科学院过程工程研究所 | Method of preparing vanadate of alkali metal from residue of aluminum powder vanadium removal of crude titanium tetrachloride |
| CN104649320B (en) * | 2013-11-20 | 2016-09-28 | 中国科学院过程工程研究所 | From crude titanic chloride aluminium powder except the method preparing alkali metal vanadate in vanadium slag |
| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
| CN108821300B (en) * | 2018-08-06 | 2021-02-09 | 东北大学 | Preparation of CaSiO from waste silicon slag3Method (2) |
| US11247270B2 (en) | 2019-01-31 | 2022-02-15 | Na Wang | Method for preparing vanadium and vanadium alloy powder from vanadium-containing materials through shortened process |
| CN114291879A (en) * | 2021-11-23 | 2022-04-08 | 攀钢集团研究院有限公司 | Preparation method of aluminum silicate |
| CN114291879B (en) * | 2021-11-23 | 2023-09-05 | 攀钢集团研究院有限公司 | Preparation method of aluminum silicate |
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