CN116287737A - Method for realizing cyclic utilization of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen - Google Patents
Method for realizing cyclic utilization of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen Download PDFInfo
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- CN116287737A CN116287737A CN202310222052.2A CN202310222052A CN116287737A CN 116287737 A CN116287737 A CN 116287737A CN 202310222052 A CN202310222052 A CN 202310222052A CN 116287737 A CN116287737 A CN 116287737A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 93
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000010936 titanium Substances 0.000 title claims abstract description 78
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 77
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 53
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000011575 calcium Substances 0.000 title claims abstract description 36
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 35
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 35
- 239000010703 silicon Substances 0.000 title claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000011593 sulfur Substances 0.000 title claims abstract description 22
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 19
- 125000004122 cyclic group Chemical group 0.000 title description 3
- 239000002893 slag Substances 0.000 claims abstract description 103
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 49
- 239000010959 steel Substances 0.000 claims abstract description 49
- 238000002386 leaching Methods 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 24
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004064 recycling Methods 0.000 claims abstract description 21
- 239000002210 silicon-based material Substances 0.000 claims abstract description 20
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 18
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 16
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 14
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 14
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 14
- 239000006227 byproduct Substances 0.000 claims abstract description 12
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 10
- 239000010440 gypsum Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000002910 solid waste Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 32
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- 235000010215 titanium dioxide Nutrition 0.000 claims description 16
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 235000021110 pickles Nutrition 0.000 abstract 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 description 33
- 239000002253 acid Substances 0.000 description 14
- 239000002699 waste material Substances 0.000 description 9
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 238000004537 pulping Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910000805 Pig iron Inorganic materials 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 1
- 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 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000002308 calcification Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HEHINIICWNIGNO-UHFFFAOYSA-N oxosilicon;titanium Chemical compound [Ti].[Si]=O HEHINIICWNIGNO-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/42—Preparation from nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
- C22B34/125—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors containing a sulfur ion as active agent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
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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
Abstract
The invention discloses a method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources, which comprises the following steps: s1, carrying out nitric acid pressure leaching on titanium-containing blast furnace slag to remove calcium element, obtaining titanium-silicon material and titanium-containing blast furnace slag pickle liquor, carrying out acidolysis and hydrolysis processes on the titanium-silicon material serving as titanium sulfate white raw material, and simultaneously obtaining a byproduct of dilute sulfuric acid; s2, crushing and grinding the vanadium-containing steel slag, and then leaching the steel slag by using dilute sulfuric acid which is a byproduct of S1 at normal pressure, and carrying out solid-liquid separation on the leached slurry to obtain a building gypsum product and vanadium-containing leaching liquid; s3, cooling and crystallizing the vanadium-containing leaching solution to separate out ferrous sulfate, and reacting the ferrous sulfate with the titaniferous blast furnace slag pickle liquor to prepare high-purity calcium sulfate and ferric nitrate, wherein the ferric nitrate is heated and decomposed to co-produce nitric acid and high-purity iron red products. The invention organically combines the two industrial solid waste resource utilization of the vanadium-containing steel slag and the titanium-containing blast furnace slag, has high comprehensive utilization rate of vanadium and titanium resources, utilizes calcium, iron and silicon, and has the advantages of low economic cost and environmental protection.
Description
Technical Field
The invention belongs to the field of comprehensive recycling of solid wastes, and particularly relates to a method for recycling titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen.
Background
The titanium-containing blast furnace slag is waste slag discharged during pig iron smelting of the blast furnace, and main chemical elements comprise titanium, iron, calcium, silicon and the like, and belongs to general industrial waste. At present, titanium-containing blast furnace slag piled up in climbing flower areas is more than 8000 ten thousand t, and increases at a speed of 360 ten thousand t/year. The titanium-containing blast furnace slag can be used in the fields of cement, building materials and the like, but valuable metal titanium, impurity elements such as calcium, silicon and the like are not effectively utilized, so that resource waste is caused.
The vanadium-containing steel slag is industrial waste slag generated in the smelting process of vanadium titano-magnetite, the vanadium content of the vanadium-containing steel slag is 1% -4%, and the vanadium-containing steel slag can be theoretically used as a vanadium extraction raw material. However, the existing form of vanadium in the steel slag is complex and extremely uneven in distribution, and the steel slag also contains a large amount of elements such as calcium, iron and silicon, so that not only is the separation and purification of vanadium affected, but also the economic cost of extracting vanadium is high, and industrial application is difficult to realize.
The domestic scientific researchers are largely researched on the recycling utilization of the titanium-containing blast furnace slag and the vanadium-containing steel slag, and the utilization method of the titanium-containing blast furnace slag comprises the following steps: (1) producing ferrotitanium alloy by an aluminothermic method and a carbothermic method; (2) recovering titanium resources by an acid leaching method and an alkali molten salt method; (3) preparing titanium tetrachloride by high-temperature carbonization-low-temperature chlorination; (4) preparing a photocatalytic degradation agent and the like. The utilization method of the vanadium-containing steel slag comprises the following steps: (1) secondary smelting to prepare high-grade vanadium slag; (2) preparing vanadium-containing pig iron by high-temperature reduction; (3) sodium roasting-leaching to extract vanadium; (4) performing calcification roasting-leaching to extract vanadium; (5) extracting vanadium by direct leaching, etc. Scientific researchers develop a large number of technical processes for extracting titanium and vanadium resources from titanium-containing blast furnace slag and vanadium-containing steel slag, but the defects of low comprehensive recovery rate, environmental pollution caused by large-scale wastewater discharge, high raw material consumption, high treatment cost and the like exist, and the large-scale application technology is still immature.
CN108359806a discloses a comprehensive treatment method of steel slag, vanadium slag and titanium white waste acid, mixing the vanadium slag, the steel slag and the titanium white waste acid, roasting, and recovering vanadium resources through water immersion-resin adsorption, wherein the vanadium yield in the whole process can reach 90%. The method is to mix and bake titanium white waste acid, vanadium slag and steel slag, so as to generate a large amount of sulfur-containing waste gas, pollute the atmosphere and increase a tail gas treatment system. Meanwhile, the titanium white waste acid contains a large amount of impurity elements such as iron, phosphorus, aluminum and the like, so that the subsequent leachate treatment cost is increased.
CN103952567B discloses a method for recovering titanium, silicon, aluminum, calcium and magnesium from titanium-containing blast furnace slag by using multistage acid leaching, and recovering useful metals such as titanium, aluminum, calcium and magnesium by using a multistage acid leaching-extraction process. The method adopts multi-stage hydrochloric acid leaching and chlorine oxidation, which not only has high requirements on equipment reliability, but also has long production flow, and is not beneficial to industrialization.
Disclosure of Invention
Aiming at the problems of long process flow, higher operation requirement and difficulty, low comprehensive recovery rate and the like of the recovery of metals from the titanium-containing blast furnace slag and the vanadium-containing steel slag in the prior art, the invention provides the method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen, which can realize the comprehensive recovery and utilization of titanium, vanadium, iron and sulfur in the titanium-containing blast furnace slag and the vanadium-containing steel slag and the co-production of nitric acid, and has the advantages of high comprehensive utilization rate of resources, no generation of new waste water and waste residues, good economic benefit and environmental protection.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for achieving cyclic utilization of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources, the method comprising the steps of:
s1, carrying out nitric acid pressure leaching on titanium-containing blast furnace slag, and removing main impurity calcium element to obtain TiO 2 The titanium-silicon material is used as a titanium sulfate white raw material to carry out acidolysis and hydrolysis processes to obtain a titanium dioxide product and active silicon, and meanwhile, the byproduct is dilute sulfuric acid with the mass concentration of 23% -27%;
s2, crushing and grinding the vanadium-containing steel slag, and then leaching the steel slag by using dilute sulfuric acid which is a byproduct of S1 at normal pressure, and carrying out solid-liquid separation on the leached slurry to obtain a building gypsum product and vanadium-containing leaching liquid;
and S3, cooling and crystallizing the vanadium-containing leaching solution obtained in S2 to separate out ferrous sulfate, carrying out precipitation reaction on the ferrous sulfate and the titanium-containing blast furnace slag pickling solution obtained in S1 to prepare high-purity calcium sulfate and ferric nitrate, and carrying out heating decomposition on the ferric nitrate to coproduce nitric acid and high-purity iron oxide red products, thereby realizing recycling of nitric acid.
Preferably, in step S1, the titanium-containing blast furnace slag is solid waste generated in the ironmaking process, and the main element mass contents thereof are as follows: tiO (titanium dioxide) 2 ：20％～25％，Fe：1.0％～2.0％，SiO 2 ：15～20％，CaO：40％～45％。
Preferably, in step S1, the titanium-containing blast furnace slag is subjected to oxidizing roasting and then nitric acid pressure leaching, so that the calcium element is activated, the leaching rate of calcium is improved, and the titanium content in the titanium-silicon material is further improved. Preferably, the roasting temperature of the titanium-containing blast furnace slag is 800-950 ℃, the roasting time is 2-4 h, the mass concentration of nitric acid adopted by nitric acid pressure leaching is 20-30%, the leaching temperature is 120-180 ℃, the solid ratio of leaching liquid is 4-6:1, and the leaching time is 2-6 h.
Preferably, in step S1, the main element content in the titanium silicon material is: tiO (titanium dioxide) 2 ：40％～45％、TFe：2.0％～4.0％、CaO：2.0％～4.0％、SiO 2 :45% -50%. The titanium-silicon material is used as a titanium sulfate white raw material and has excellent acidolysis performance.
Preferably, in the step S1, the byproduct dilute sulfuric acid of the sulfuric acid method titanium white contains the following main elements: h + 5 to 8mol/L, ti, 1.0 to 3.0g/L, fe, 2.0 to 5.0g/L, ca, 0.1 to 0.3g/L, mg, 0.2 to 0.8g/L, al and 0.1 to 0.5g/L. The byproduct dilute sulfuric acid has low impurity element content, and can be used for acid leaching of vanadium-containing steel slag.
Preferably, in step S2, the vanadium-containing steel slag is solid waste generated in the steelmaking process, and the main element mass content of the vanadium-containing steel slag is: v (V) 2 O 5 ：2.5％～3.0％，Fe：20.0％～25.0％，SiO 2 ：5％～10％，CaO：35％～40％。
Preferably, in the step S2, the grain size of the crushed and ground vanadium-containing steel slag is 300-400 meshes, and the sulfuric acid atmospheric leaching mode is as follows: adding water into the vanadium-containing steel slag to pulp, and then slowly dripping the dilute sulfuric acid solution of the S1 byproduct. The grain size and the acid leaching mode of the vanadium-containing steel slag need to be controlled, so that the leaching rate of vanadium and iron and the quality of building gypsum are improved.
Preferably, in the step S2, when the vanadium-containing steel slag is leached, the mass ratio of the dilute sulfuric acid to the vanadium-containing steel slag is 6-8:1, the leaching temperature is 30-70 ℃, and the leaching time is 3-6 h.
Preferably, in step S3, the temperature at which the ferric nitrate is thermally decomposed is 200 to 300 ℃. If the calcium nitrate obtained in the step S1 is pyrolyzed, the pyrolysis temperature is 700-800 ℃. Compared with the prior art, the method converts the calcium nitrate which is difficult to decompose into the ferric nitrate which is easy to decompose, reduces the temperature of pyrolysis reaction, and is convenient for preparing nitric acid subsequently.
Particularly, the acid used for acid leaching of the vanadium-containing steel slag in the S2 is waste dilute sulfuric acid produced in the process of preparing titanium dioxide from the titanium-containing blast furnace slag in the S1, so that the acid usage amount in the whole process is reduced.
According to the invention, two industrial solid wastes of titanium-containing blast furnace slag and vanadium-containing steel slag are organically combined, vanadium, titanium, calcium, sulfur, silicon and iron resources are comprehensively recovered, and meanwhile, the recycling of nitrogen is realized. Compared with the prior art, the method has the following advantages:
1) In the step S1, the titanium-containing blast furnace slag is roasted and activated, so that the activity of calcium is improved, and the leaching of the calcium is facilitated.
2) The titanium-containing blast furnace slag in the step S1 adopts the nitric acid impurity removal-sulfuric acid acidolysis sectional treatment procedure, so that the acid usage amount of the whole process is reduced, and no new waste slag is generated in the process. The titanium-containing blast furnace slag is subjected to pre-impurity removal, the content of dilute sulfuric acid impurity elements generated in the hydrolysis process is low, the dilute sulfuric acid impurity elements can be directly used for the acid leaching vanadium-leaching process of the vanadium-containing steel slag without treatment, and the production flow is simplified.
3) The byproduct gypsum produced in the leaching process of the vanadium-containing steel slag in the step S2 has higher whiteness, low iron and aluminum content, and component content similar to that of natural gypsum, and has wide application.
4) And S3, carrying out precipitation reaction on calcium nitrate produced by the titanium-containing blast furnace slag and ferrous sulfate produced by the vanadium-containing steel slag to obtain high-purity calcium sulfate and high-purity iron oxide red, and simultaneously, co-producing nitric acid for recycling.
In conclusion, the invention organically combines the two industrial solid waste resource utilization of the vanadium-containing steel slag and the titanium-containing blast furnace slag, and the dilute sulfuric acid generated in the titanium extraction stage of the titanium-containing blast furnace slag is used for extracting vanadium from the vanadium-containing steel slag, so that the recovery rate of titanium can reach 85%, the recovery rate of vanadium can reach 90%, the recovery rate of iron can reach 95%, and the utilization rate of sulfur can reach 95%. Not only is the comprehensive utilization rate of vanadium and titanium resources high, but also calcium, iron and silicon are utilized, and the method has the advantages of low economic cost and environmental protection.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the method for realizing the recycling of resources such as titanium, vanadium, iron, calcium, silicon, sulfur, nitrogen and the like.
Detailed Description
The technical solutions and the technical problems to be solved in the embodiments of the present invention will be described below in conjunction with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, of the embodiments of the present patent.
Comparative example 1
1) The titanium-containing blast furnace slag is not roasted, is directly ground to have the average granularity of 0.06mm, and then the ground titanium-containing blast furnace slag and nitric acid with the concentration of 20% are poured into a pressurized reaction kettle, the mass ratio of the titanium-containing blast furnace slag to the nitric acid solution is 1:5, and the reaction is carried out for 2 hours at 160 ℃. After the reaction is finished, solid-liquid separation is carried out, the obtained filter residue is titanium-silicon material, and TiO thereof 2 The content of SiO is 33.54 percent 2 The content is 30.12 percent, and the content of calcium in the filtrate is 13.15g/l.
Because the titanium-containing blast furnace slag is not roasted, the leaching rate of calcium is lower, the quality of titanium-silicon materials is poor, and the next experiment is unnecessary.
Comparative example 2
1) Roasting titanium-containing blast furnace slag blank at 800 ℃ for 2 hours, grinding to an average particle size of 0.06mm, then pouring the ground titanium-containing blast furnace slag clinker and nitric acid with 20% concentration into a pressurized reaction kettle, and reacting the titanium-containing blast furnace slag clinker and the nitric acid solution for 2 hours at 160 ℃. After the reaction is finished, solid-liquid separation is carried out, the obtained filter residue is titanium-silicon material, and TiO thereof 2 The content of SiO is 43.54 percent 2 The content is 40.12 percent, and the content of calcium in the filtrate is 22.15g/l, which is taken as solution 1;
2) Adding 100g of titanium-silicon material into a 500ml beaker, then adding 80% sulfuric acid to carry out acidolysis at 160 ℃, wherein the mass ratio of the titanium-silicon material to the sulfuric acid solution is 1:3, curing, cooling and settling after acidolysis, and carrying out solid-liquid separation to obtain filtrate which is titanyl sulfate solution and filter residues which are active silicon;
3) Hydrolyzing the obtained titanyl sulfate solution at 90 ℃ for 2 hours, and carrying out solid-liquid separation after the reaction is finished to obtain filter residue 1 and filtrate 2, wherein the filter residue 1 is a hydrated titanium dioxide product, and the filtrate 2 is dilute sulfuric acid with the concentration of 25.21%;
4) 100g of vanadium-containing steel slag crushed to an average particle size of 0.04mm is taken and added with 500mlAnd adding the filtrate 2 into the flask, and stirring and reacting for 3 hours at the temperature of 40 ℃, wherein the mass ratio of the vanadium-containing steel slag to the filtrate 2 is 8:1. After the reaction is finished, solid-liquid separation is carried out, and the obtained filter residue is a building gypsum product, caSO 4 The content is 75.31%, the obtained filtrate has low iron content, and ferrous sulfate can not be obtained through cooling crystallization.
The leaching rate of vanadium and iron is lower because no water is added into the steel slag containing vanadium for pulping. The vanadium-containing steel slag is directly mixed with the filtrate 2, so that the speed of generating calcium sulfate is high, and the iron-containing phase is wrapped, so that the iron leaching rate is low.
Example 1
The embodiment discloses a method for recycling resources such as titanium, vanadium, iron, calcium, silicon, sulfur, nitrogen and the like, wherein a flow chart is shown in fig. 1, and the method specifically comprises the following steps:
1) Roasting titanium-containing blast furnace slag blank at 800 ℃ for 2 hours, grinding to an average particle size of 0.06mm, then pouring the ground titanium-containing blast furnace slag clinker and nitric acid with 20% concentration into a pressurized reaction kettle, and reacting the titanium-containing blast furnace slag clinker and the nitric acid solution for 2 hours at 160 ℃. After the reaction is finished, solid-liquid separation is carried out, the obtained filter residue is titanium-silicon residue, and TiO (titanium-silicon oxide) is used as the filter residue 2 The content of SiO is 43.54 percent 2 The content is 40.12 percent, and the content of calcium in the filtrate is 22.15g/l, which is taken as solution 3;
2) Adding 100g of titanium-silicon material into a 500ml beaker, then adding 80% sulfuric acid to carry out acidolysis at 160 ℃, wherein the mass ratio of the titanium-silicon material to the sulfuric acid solution is 1:3, curing, cooling and settling after acidolysis, and carrying out solid-liquid separation to obtain filtrate which is titanyl sulfate solution and filter residues which are active silicon;
3) Hydrolyzing the obtained titanyl sulfate solution at 90 ℃ for 2 hours, and carrying out solid-liquid separation after the reaction is finished to obtain filter residue 2 and filtrate 4, wherein the filter residue 2 is a hydrated titanium dioxide product, and the filtrate 4 is dilute sulfuric acid with the concentration of 25.21%;
4) 100g of vanadium-containing steel slag with the average granularity of 0.04mm is taken and crushed into a 500ml flask, a small amount of water is added for pulping, then filtrate 4 is slowly dripped into the flask, stirring reaction is carried out for 3 hours at 40 ℃, and the mass ratio of the vanadium-containing steel slag to the filtrate 4 is 8:1. After the reaction is finishedPerforming solid-liquid separation to obtain filter residue as building gypsum product, and CaSO 4 The content is 90.03%, and the obtained filtrate is cooled and crystallized to obtain ferrous sulfate and vanadium-containing liquid;
5) And (3) adding 15g of ferrous sulfate into a 500ml beaker while stirring 200ml of solution 3, carrying out solid-liquid separation after the reaction is finished at the reaction temperature of 35 ℃ for 1h, wherein the content of calcium sulfate in the obtained filter residue is 98.5%, and the content of ferric oxide obtained by decomposing the obtained filtrate at low temperature is 98.2%.
Example 2
The embodiment discloses a method for realizing the recycling of resources such as titanium, vanadium, iron, calcium, silicon, sulfur, nitrogen and the like, which specifically comprises the following steps:
1) Roasting titanium-containing blast furnace slag blank at 850 ℃ for 1h, grinding to an average particle size of 0.06mm, then pouring the ground titanium-containing blast furnace slag clinker and nitric acid with the concentration of 25% into a pressurized reaction kettle, and reacting the titanium-containing blast furnace slag clinker and nitric acid solution for 2h at 180 ℃. After the reaction is finished, solid-liquid separation is carried out, the obtained filter residue is titanium-silicon material, and TiO thereof 2 The content is 44.58 percent, siO 2 The content is 42.43%, and the calcium content in the filtrate is 25.76g/l, which is taken as solution 5;
2) Adding 100g of titanium-silicon material into a 500ml beaker, then adding 90% sulfuric acid to carry out acidolysis at 170 ℃, wherein the mass ratio of the titanium-silicon material to the sulfuric acid solution is 1:2, curing, cooling and settling after acidolysis, and carrying out solid-liquid separation to obtain filtrate which is titanyl sulfate solution and filter residues which are active silicon;
3) Hydrolyzing the obtained titanyl sulfate solution at 90 ℃ for 2 hours, and carrying out solid-liquid separation after the reaction is finished to obtain filter residue 3 and filtrate 6, wherein the filter residue 3 is a hydrated titanium dioxide product, and the filtrate 6 is 26.01% dilute sulfuric acid;
4) 100g of vanadium-containing steel slag with the average granularity of 0.04mm is taken and crushed into a 500ml flask, a small amount of water is added for pulping, then filtrate 6 is slowly dripped into the flask, stirring reaction is carried out for 3 hours at the temperature of 60 ℃, and the mass ratio of the vanadium-containing steel slag to the filtrate 6 is 8:1. After the reaction is finished, solid-liquid separation is carried out, and the obtained filter residue is a building gypsum product, caSO 4 The content is 92.34 percent, theCooling and crystallizing the filtrate to obtain ferrous sulfate and vanadium-containing liquid;
5) And (3) adding 18g of ferrous sulfate into a 500ml beaker while stirring 200ml of solution 5, carrying out solid-liquid separation after the reaction is finished at the reaction temperature of 35 ℃ for 2 hours, wherein the content of calcium sulfate in the obtained filter residue is 98.9%, and the content of ferric oxide obtained by decomposing the obtained filtrate at low temperature is 99.1%.
Example 3
The embodiment discloses a method for realizing the recycling of resources such as titanium, vanadium, iron, calcium, silicon, sulfur, nitrogen and the like, which specifically comprises the following steps:
1) Roasting titanium-containing blast furnace slag blank at 900 ℃ for 2 hours, grinding to an average particle size of 0.06mm, then pouring the ground titanium-containing blast furnace slag clinker and nitric acid with 20% concentration into a pressurized reaction kettle, and reacting the titanium-containing blast furnace slag clinker and the nitric acid solution for 2 hours at 160 ℃. After the reaction is finished, solid-liquid separation is carried out, the obtained filter residue is titanium-silicon material, and TiO thereof 2 The content is 44.15 percent, siO 2 The content is 40.92%, and the calcium content in the filtrate is 24.36g/l, which is used as solution 7;
2) Adding 100g of titanium-silicon material into a 500ml beaker, then adding 85% sulfuric acid to carry out acidolysis at 180 ℃, wherein the mass ratio of the titanium-silicon material to the sulfuric acid solution is 1:2.5, curing, cooling and settling after acidolysis, and carrying out solid-liquid separation to obtain filtrate which is titanyl sulfate solution, wherein the obtained filter residue is active silicon;
3) Hydrolyzing the obtained titanyl sulfate solution at 95 ℃ for 2 hours, and performing solid-liquid separation after the reaction is finished to obtain filter residue 4 and filtrate 8, wherein the filter residue 4 is a hydrated titanium dioxide product, and the filtrate 8 is 26.32% dilute sulfuric acid;
4) 100g of vanadium-containing steel slag with the average granularity of 0.04mm is taken and crushed into a 500ml flask, a small amount of water is added for pulping, then filtrate 8 is slowly dripped into the flask, stirring reaction is carried out for 4 hours at 80 ℃, and the mass ratio of the vanadium-containing steel slag to the filtrate 8 is 8:1. After the reaction is finished, solid-liquid separation is carried out, and the obtained filter residue is a building gypsum product, caSO 4 The content is 94.16%, and the obtained filtrate is cooled and crystallized to obtain ferrous sulfate and vanadium-containing liquid;
5) And (3) adding 20g of ferrous sulfate into a 500ml beaker while stirring 200ml of solution 7, carrying out solid-liquid separation after the reaction is finished at the reaction temperature of 40 ℃ for 1.5h, wherein the content of calcium sulfate in the obtained filter residue is 99.3%, and the content of ferric oxide obtained by decomposing the obtained filtrate at low temperature is 99.2%.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A method for recycling titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources, the method comprising the steps of:
s1, carrying out nitric acid pressure leaching on titanium-containing blast furnace slag, and removing main impurity calcium element to obtain TiO 2 The titanium-silicon material is used as a titanium sulfate white raw material to carry out acidolysis and hydrolysis processes to obtain a titanium dioxide product and active silicon, and meanwhile, the byproduct is dilute sulfuric acid with the mass concentration of 23% -27%;
s2, crushing and grinding the vanadium-containing steel slag, and then leaching the steel slag by using dilute sulfuric acid which is a byproduct of S1 at normal pressure, and carrying out solid-liquid separation on the leached slurry to obtain a building gypsum product and vanadium-containing leaching liquid;
and S3, cooling and crystallizing the vanadium-containing leaching solution obtained in S2 to separate out ferrous sulfate, carrying out precipitation reaction on the ferrous sulfate and the titanium-containing blast furnace slag pickling solution obtained in S1 to prepare high-purity calcium sulfate and ferric nitrate, and carrying out heating decomposition on the ferric nitrate to coproduce nitric acid and high-purity iron oxide red products, thereby realizing recycling of nitric acid.
2. The method for recycling titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in step S1, the titanium-containing blast furnace slag is solid waste generated in the iron-making process, and the main element mass contents are as follows: tiO (titanium dioxide) 2 ：20％～25％，Fe：1.0％～2.0％，SiO 2 ：15～20％，CaO：40％～45％。
3. The method for recycling titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in step S1, the titanium-containing blast furnace slag is subjected to oxidizing roasting and then nitric acid pressure leaching.
4. The method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 3, wherein the roasting temperature of the titanium-containing blast furnace slag is 800-950 ℃, the roasting time is 2-4 h, the nitric acid pressure leaching adopts nitric acid with the mass concentration of 20-30%, the leaching temperature is 120-180 ℃, the leaching solution solid ratio is 4-6:1, and the leaching time is 2-6 h.
5. The method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in the step S1, the content of main elements of the byproduct dilute sulfuric acid of the titanium white by the sulfuric acid method is as follows: h + :5～8mol/L、Ti:1.0～3.0g/L、Fe:2.0～5.0g/L、Ca:0.1～0.3g/L、Mg:0.2～0.8g/L、Al:0.1～0.5g/L。
6. The method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in the step S2, the grain size of the vanadium-containing steel slag after being crushed and ground is 300-400 meshes, and the sulfuric acid normal pressure leaching mode is as follows: adding water into the vanadium-containing steel slag to pulp, and then slowly dripping the dilute sulfuric acid solution of the S1 byproduct.
7. The method for realizing the recycling of titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in the step S2, when the vanadium-containing steel slag is leached, the mass ratio of dilute sulfuric acid to the vanadium-containing steel slag is 6-8:1, the leaching temperature is 30-70 ℃, and the leaching time is 3-6 h.
8. The method for recycling titanium, vanadium, iron, calcium, silicon, sulfur and nitrogen resources according to claim 1, wherein in step S3, the temperature of the thermal decomposition of ferric nitrate is 200-300 ℃.
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