CN117344132A - Method for preparing silicon-chromium alloy from lithium ore and enriching lithium mixture - Google Patents
Method for preparing silicon-chromium alloy from lithium ore and enriching lithium mixture Download PDFInfo
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- CN117344132A CN117344132A CN202311647000.6A CN202311647000A CN117344132A CN 117344132 A CN117344132 A CN 117344132A CN 202311647000 A CN202311647000 A CN 202311647000A CN 117344132 A CN117344132 A CN 117344132A
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- 239000000203 mixture Substances 0.000 title claims abstract description 146
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 125
- 229910000599 Cr alloy Inorganic materials 0.000 title claims abstract description 52
- 239000000788 chromium alloy Substances 0.000 title claims abstract description 52
- DYRBFMPPJATHRF-UHFFFAOYSA-N chromium silicon Chemical compound [Si].[Cr] DYRBFMPPJATHRF-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 60
- 239000002893 slag Substances 0.000 claims abstract description 50
- 229910000604 Ferrochrome Inorganic materials 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- 238000006722 reduction reaction Methods 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003546 flue gas Substances 0.000 claims abstract description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 13
- 239000011575 calcium Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 49
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 47
- 229910052642 spodumene Inorganic materials 0.000 claims description 43
- 239000000571 coke Substances 0.000 claims description 27
- 239000000292 calcium oxide Substances 0.000 claims description 25
- 235000012255 calcium oxide Nutrition 0.000 claims description 25
- 239000011651 chromium Substances 0.000 claims description 24
- 235000019738 Limestone Nutrition 0.000 claims description 3
- 239000006028 limestone Substances 0.000 claims description 3
- 229910052570 clay Inorganic materials 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 229910052629 lepidolite Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- -1 alkali metal salts Chemical class 0.000 abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 241001062472 Stokellia anisodon Species 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 19
- 229910052748 manganese Inorganic materials 0.000 description 19
- 239000007788 liquid Substances 0.000 description 18
- PYLLWONICXJARP-UHFFFAOYSA-N manganese silicon Chemical compound [Si].[Mn] PYLLWONICXJARP-UHFFFAOYSA-N 0.000 description 18
- 229910000676 Si alloy Inorganic materials 0.000 description 17
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 13
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 13
- 239000012535 impurity Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 11
- 229910052804 chromium Inorganic materials 0.000 description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 10
- 229910052808 lithium carbonate Inorganic materials 0.000 description 10
- 229910003002 lithium salt Inorganic materials 0.000 description 9
- 159000000002 lithium salts Chemical class 0.000 description 9
- 230000002349 favourable effect Effects 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 229910018643 Mn—Si Inorganic materials 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000005266 casting Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 229910019974 CrSi Inorganic materials 0.000 description 4
- 229910018068 Li 2 O Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 229910017028 MnSi Inorganic materials 0.000 description 3
- 229910018540 Si C Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910003849 O-Si Inorganic materials 0.000 description 2
- 229910003872 O—Si Inorganic materials 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001180 sulfating effect Effects 0.000 description 2
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 2
- 229910052644 β-spodumene Inorganic materials 0.000 description 2
- 229910010100 LiAlSi Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 229910008458 Si—Cr Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052643 α-spodumene Inorganic materials 0.000 description 1
Classifications
-
- 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
- C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
- C22B4/06—Alloys
-
- 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
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- 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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- 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
- C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
- C22B4/02—Light metals
-
- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of nonferrous metal metallurgy, in particular to a method for preparing a silicon-chromium alloy from lithium ores and enriching a lithium mixture, which comprises the following steps of (1) mixing the lithium ores, high-carbon ferrochrome, a carbon reducing agent and a calcium additive to obtain a mixture; (2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace for high-temperature reduction reaction, smelting to obtain silicon-chromium alloy and high-aluminum slag, and recovering a lithium mixture in a flue gas cooling system of the submerged arc furnace. The invention has the beneficial effects that: the lithium ore is adopted to smelt the silicon-chromium alloy, the lithium mixture is enriched, the slag is the blast-furnace slag, lithium, silicon and aluminum in the lithium ore gangue are comprehensively utilized, the enriched lithium mixture has high lithium content, conditions are provided for the subsequent high-efficiency production of alkali metal salts such as lithium, the environment pollution is avoided, and the production cost of the alkali metal salts such as lithium is reduced.
Description
Technical Field
The invention relates to the technical field of nonferrous metal metallurgy, in particular to a method for preparing a silicon-chromium alloy from lithium ores and enriching a lithium mixture.
Background
Lithium is an important strategic resource, and with the rapid development of new energy automobiles, lithium is widely used as a positive electrode material of high energy density lithium ion batteries.
At present, the technology for producing the lithium carbonate in China generally adopts a sulfuric acid acidification roasting method, namely spodumene is used as a raw material, and the technology comprises the technological processes of calcination transformation, acidification roasting, leaching, purification, lithium precipitation and the like. However, every 1 ton of lithium salt is produced, tens of tons of high-alumina-silica leaching residues are produced, and serious harm is caused to the environment. Therefore, the process for producing the lithium carbonate by comprehensively utilizing the lithium ore in a recycling way is very important.
The invention patent application No. 201080065025.X discloses a method of manufacturing lithium carbonate, the method comprising: calcining the alpha spodumene ore to produce beta spodumene; then cooling, ball milling, mixing with sulfuric acid, transferring into a sulfating kiln, and sulfating beta spodumene at high temperature; leaching the sulfated beta spodumene with water to produce a lithium sulfate solution; and then, through a series of purification and impurity removal measures, finally obtaining lithium carbonate and sodium sulfate.
The invention patent application with the application number of 20110000790. X discloses a method for producing lithium carbonate and lithium hydroxide, spodumene concentrate is subjected to high-temperature roasting at 1050-1100 ℃, cooling, fine grinding, adding 98% of concentrated sulfuric acid, acidizing and roasting at 250-300 ℃, extracting by a wet method to remove calcium and magnesium impurities, evaporating, concentrating and press-filtering to obtain a lithium sulfate solution, thereby obtaining lithium carbonate; lithium hydroxide can also be obtained by adding barium hydroxide to the lithium carbonate mother liquor.
The above Chinese patent application adopts sulfuric acid method to extract lithium from spodumene, the obtained lithium exists in the form of lithium salt such as lithium carbonate and lithium hydroxide, aluminum and silicon in spodumene are filtered and enter slag, a large amount of leached slag is difficult to be dissolved, and serious pollution is caused to the environment.
Disclosure of Invention
In view of the above, the invention provides a method for preparing a silicon-chromium alloy from lithium ores and enriching a lithium mixture, which aims to solve a series of problems of high pollution, high energy consumption, low recovery rate, low comprehensive utilization rate of leaching residues and the like in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: there is provided a method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture, comprising the steps of:
(1) Mixing lithium ore, high-carbon ferrochrome, a carbon reducing agent and a calcium additive to obtain a mixture; the high-carbon ferrochrome comprises the following elements in percentage by mass: cr is more than or equal to 55%, fe is more than or equal to 30%, C is more than or equal to 6% and less than or equal to 10%; the high-carbon ferrochrome can be replaced by chrome ore, and the chrome ore comprises the following components in percentage by mass: cr (Cr) 2 O 3 More than or equal to 38 percent and the mass ratio of Cr/Fe is more than 1.68.
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace for high-temperature reduction reaction, wherein the temperature of the high-temperature reduction reaction is 1000-2200 ℃, the reaction time is 1-24 h, smelting to obtain silicon-chromium alloy and blast-aluminum slag, and recovering the lithium mixture in a flue gas cooling system of the submerged arc furnace.
The key conception of the technical scheme is as follows: and taking high-carbon ferrochrome as an auxiliary agent, reducing and volatilizing Li in the lithium ore at a high temperature, condensing and enriching, combining Si and Cr to form Si-Cr alloy, and enriching Al in slag. The lithium ore and the high-carbon ferrochrome are used for smelting the silicon-chromium alloy, the lithium mixture is enriched, the slag is high-aluminum slag, lithium, silicon and aluminum in the lithium ore gangue are comprehensively utilized, and the enriched lithium mixture is high in lithium content, so that conditions are provided for the subsequent efficient production of alkali metal salts such as lithium, environmental pollution is avoided, and the production cost of the alkali metal salts such as lithium is reduced.
Preferably, in the method for preparing the silicon-chromium alloy and enriching the lithium mixture from the lithium ore, the lithium ore is one or more of spodumene, lepidolite and clay type lithium ore which are mixed in any proportion.
Preferably, in the method for preparing the silicon-chromium alloy from the lithium ore and enriching the lithium mixture, the high-carbon ferrochrome is one or a mixture of a plurality of brands in GB/T5683-2008 in any proportion.
The GB/T5683-2008 comprises the following marks: feCr67C6.0, feCr55C6.0, feCr67C9.5, feCr55C10.0.
Preferably, in the method for preparing the silicon-chromium alloy from the lithium ore and enriching the lithium mixture, the carbon reducing agent is one or a mixture of two of semi-coke and coke.
Preferably, in the method for preparing the silicon-chromium alloy from the lithium ore and enriching the lithium mixture, the calcium additive is one or two of calcium-containing substances such as quicklime, limestone and the like which are mixed in any proportion.
Preferably, in the method for preparing the silicon-chromium alloy from the lithium ore and enriching the lithium mixture, the mass ratio of the lithium ore in the mixture in the step (1) to C in the carbon reducer is 1-5:1; the molar ratio of Si in the lithium ore to Cr in the high-carbon ferrochrome is 1-4:1; the addition amount of the calcium additive is 5-20% of the total mass of the lithium ore, the carbon reducer and the high-carbon ferrochrome.
As can be seen from the above description, the above raw material ratio enables C to fully reduce SiO in lithium ore 2 And Li (lithium) 2 O, the reduced Si and chromium are combined into alloy phase, so that Si in the silicon-chromium alloy is more than or equal to 40%, cr is more than or equal to 30%, and calcium additive and Al in lithium ore are added 2 O 3 The formation of high-aluminum slag damages the lithium ore structure, and Li is more easily reduced.
The quality of the silicon-chromium alloy prepared by the method for preparing the silicon-chromium alloy from the lithium ore and enriching the lithium mixture meets the national standard (GB/T4009-2008) requirements: si more than or equal to 40%, cr more than or equal to 30%, C0.02% -1.0%, P0.02% -0.04%, S0.01%. Al is contained in the obtained blast-furnace slag 2 O 3 More than or equal to 55 percent. The reduction rate of Li is more than or equal to 95%, the comprehensive recovery rate of Li is more than or equal to 85.0%, the recovery rate of silicon in lithium ore is more than or equal to 90%, the recovery rate of Al is more than or equal to 85%, and the recovery rate of chromium in high-carbon ferrochrome is more than or equal to 92%.
The reaction process involved in the invention is as follows:
2C+SiO 2 →Si+2CO （1）
Cr 7 C 3 + 7Si→ 7CrSi + 3C （2)
C+O 2 →CO 2 （3）
Cr 7 C 3 +10Si→ 7CrSi +3SiC (4)
LiAlSi 2 0 6 +C+Cr 7 C 3 →CrSi+Al 2 0 3 +Li(g)+ CO(g) (5)
Cr 7 C 3 +7Si0 2 +14C → 7CrSi+17CO(g) (6)
4Li+O 2 = 2Li 2 O (7)
CaO+Al 2 0 3 = CaO·Al 2 0 3 (8)
Li+H 2 O ＝LiOH+0 .5H 2 (9)
Li 2 O+H 2 O＝2LiOH (10)
the invention has the beneficial effects that: the invention uses high carbon ferrochrome carbothermic reduction to prepare the silicon-chromium alloy and enrich the lithium mixture, and has the following obvious advantages: by using SiO as the main constituent in lithium ores 2 As a silicon source for smelting the silicon-chromium alloy; chromium has a higher melting point and boiling point than other metals such as manganese, iron and the like, and the high temperature is more favorable for destroying the structure of lithium ores to lead Li to be reduced and volatilized during smelting, and meanwhile, the chromium metal has low high-temperature burning loss, enters less smoke dust and is more favorable for enriching Li. Chromium is easier to combine with silicon than iron, is favorable for reaction, and inhibits volatilization of SiO; the high-carbon ferrochrome contains about 10% of carbon, so that the consumption of a carbonaceous reducing agent is reduced; high-carbon ferrochrome contains less impurities, and Al in slag 2 O 3 The content is high; the high-carbon ferrochrome is used as an additive, and C is used as a reducing agent, so that Al-O-Si bonds in spodumene are easily broken, lithium is volatilized out to be enriched in smoke dust, the grade of lithium is greatly improved, the preparation of lithium salts such as lithium carbonate is facilitated, the production cost of the lithium salts is reduced, and the problem of large slag quantity in the traditional lithium salt production is solved.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture in accordance with an embodiment of the present invention.
Detailed Description
The invention is further described in connection with the accompanying drawings and the specific embodiments, but the scope of the invention is not limited to the description.
Example 1
Referring to fig. 1, a method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture comprises the following specific steps:
(1) Mixing spodumene, high-carbon ferrochrome, semi-coke and quick lime (calcium oxide) to obtain a mixture;
the specific proportioning is as follows: the mass ratio of spodumene to C in semi coke is 3.5:1; the molar ratio of Si in the epidesmine to Cr in the high-carbon ferrochrome is 2.5:1; the mass of the quicklime is 8% of the total mass of the other three materials (spodumene, semi-coke and high-carbon ferrochrome), and the ingredients are prepared;
the granularity of the semi-coke is 25mm, the high-carbon ferrochrome is in a 20mm block shape, the brand of the high-carbon ferrochrome is FeCr55C10, specifically, the high-carbon ferrochrome contains Cr55.20 percent and C10 percent, and spodumene is in a 20-100mm block shape, and the crushing treatment is not needed.
Spodumene composition analysis is shown in table 1;
TABLE 1 spodumene composition table
| Composition of the components | Li 2 O | SiO 2 | Al 2 O 3 | K 2 O | Na 2 O | CaO | MgO | Fe 2 O 3 | Rb 2 O | Cs 2 O |
| Content% | 5.85 | 61.00 | 20.80 | 0.75 | 0.53 | 0.70 | 0.20 | 2.10 | 0.02 | / |
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1650 ℃, and smelting for 8 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce the silicon-chromium alloy liquid and the high-aluminum slag. And discharging the liquid silicon-chromium alloy and the high-aluminum slag into a ladle, decarburizing the liquid silicon-chromium alloy, and casting in a mould. And (5) crushing and packaging the cooled silicon-chromium alloy, and selling slag.
The components of the obtained silicon-chromium alloy are shown in Table 2, and the components of the blast-furnace slag are shown in Table 3. The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in Table 4.
TABLE 2 silicon-chromium alloy composition table
| Composition of the components | Si | Cr | C | P | S |
| Content% | 44.8 | 33.2 | 0.08 | 0.02 | 0.03 |
TABLE 3 blast-furnace slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | CrSi | MgO | Impurity(s) |
| Content (%) | 55.79 | 31.25 | 8.05 | 1.14 | 1.10 | 2.67 |
TABLE 4 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Cr | Fe |
| Content (%) | 31.58 | 17.01 | 41.20 | 2.83 | 0.39 | 2.8 | 2.14 | 2.05 |
Example 2
A method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture, which comprises the following specific steps:
(1) Mixing spodumene, high-carbon ferrochrome, semi-coke and quicklime to obtain a mixture;
the specific proportioning is as follows: proportioning according to the mass ratio of spodumene to C in semi-coke of 3:1 and the molar ratio of Si in spodumene to Cr in high-carbon ferrochrome of 2:1, wherein the mass of quicklime is 5% of the total mass of the other three materials (spodumene, semi-coke and high-carbon ferrochrome);
the granularity of the semi-coke is 25mm, the high-carbon ferrochrome is 30mm block, the brand of the high-carbon ferrochrome is FeCr55C10, and the spodumene is 20-100mm block, and the crushing treatment is not needed. Spodumene composition analysis is shown in table 5;
TABLE 5 spodumene composition table
| Composition of the components | Li 2 O | SiO 2 | Al 2 O 3 | K 2 O | Na 2 O | CaO | MgO | Fe 2 O 3 | Rb 2 O | Cs 2 O |
| Content% | 3.55 | 71.50 | 18.14 | 0.55 | 0.38 | 0.50 | 0.08 | 0.96 | 0.027 | 0.0058 |
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1750 ℃, and smelting for 8 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce the silicon-chromium alloy liquid and the high-aluminum slag. And discharging the liquid silicon-chromium alloy and the high-aluminum slag into a ladle, decarburizing the liquid silicon-chromium alloy, and casting in a mould. And (5) crushing and packaging the cooled silicon-chromium alloy, and selling slag.
The composition of the silicon-chromium alloy is shown in Table 6, and the composition of the blast-furnace slag is shown in Table 7.
The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in Table 8.
TABLE 6 silicon-chromium alloy composition table
| Composition of the components | Si | Cr | C | P | S |
| Content% | 43.2 | 34.65 | 0.05 | 0.02 | 0.01 |
TABLE 7 blast-furnace slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | CrSi | MgO | Impurity(s) |
| Content (%) | 55.18 | 29.63 | 10.89 | 3.74 | 0.1 | 0.46 |
TABLE 8 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Cr | Fe |
| Content (%) | 22.80 | 27.67 | 42.30 | 2.85 | 0.74 | 0.93 | 2.12 | 0.59 |
Example 3
A method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture, which comprises the following specific steps:
(1) Mixing spodumene, high-carbon ferrochrome, coke and limestone to obtain a mixture;
the specific proportioning is as follows: mixing according to the mass ratio of spodumene to C in coke of 2.5:1 and the molar ratio of Si in spodumene to Cr in high-carbon ferrochrome of 2.5:1, wherein the mass of quicklime is 6% of the total mass of the other three materials (spodumene, coke and high-carbon ferrochrome);
the granularity of the coke is 25mm, the fixed carbon content in the coke is more than or equal to 86%, the high carbon ferrochrome is 30mm block, the brand of the high carbon ferrochrome is FeCr55C10, and spodumene is 20-100mm block, and the crushing treatment is not needed. Spodumene composition analysis is shown in table 9;
TABLE 9 spodumene composition table
| Composition of the components | Li 2 O | SiO 2 | Al 2 O 3 | K 2 O | Na 2 O | CaO | MgO | Fe 2 O 3 | Rb 2 O | Cs 2 O |
| Content% | 3.64 | 70.5 | 20.14 | 0.62 | 0.38 | 0.50 | 0.08 | 0.96 | 0.026 | 0.0049 |
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1850 ℃, and smelting for 4 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce the silicon-chromium alloy liquid and the high-aluminum slag. And discharging the liquid silicon-chromium alloy and the high-aluminum slag into a ladle, decarburizing the liquid silicon-chromium alloy, and casting in a mould. And (5) crushing and packaging the cooled silicon-chromium alloy, and selling slag.
The composition of the silicon-chromium alloy is shown in Table 10, and the composition of the blast furnace slag is shown in Table 11.
The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in Table 12.
TABLE 10 silicon-chromium alloy composition table
| Composition of the components | Si | Cr | C | P | S |
| Content% | 43.3 | 33.35 | 0.04 | 0.02 | 0.01 |
TABLE 11 blast-furnace slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | CrSi | MgO | Impurity(s) |
| Content (%) | 55.02 | 31.31 | 1.37 | 2.67 | 1.32 | 8.29 |
Table 12 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Cr | Fe |
| Content (%) | 34.45 | 13.40 | 41.31 | 5.96 | 0.98 | 0.69 | 2.37 | 0.84 |
Comparative example 1
A method for preparing manganese-silicon alloy from lithium ore and enriching lithium comprises the following specific steps:
other conditions were similar to example 1 except that the high carbon ferrochrome was changed to manganese ore, the composition of which was as follows: mn 34.4%, siO 2 15.69%，Fe 6.4%，Al 2 O 3 5%，CaO 9.07%，MgO 9%。
(1) Crushing lithium ore, manganese ore, a carbon reducing agent and a calcium additive, and then proportioning to obtain a mixture;
the specific proportioning is as follows: mixing according to the mass ratio of spodumene to C in semi-coke of 3.5:1 and the molar ratio of Si in spodumene to Mn in manganese ore of 2.5:1, wherein the mass of quicklime is 8% of the total mass of the other three materials (spodumene, semi-coke and manganese ore);
the granularity of the semi-coke is 25mm, the manganese ore is 30mm blocky, the spodumene is 20-100mm blocky, and the crushing treatment is not needed. Spodumene composition analysis is shown in table 5;
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1650 ℃, and smelting for 8 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce manganese-silicon alloy liquid and high-aluminum slag. And discharging the liquid Mn-Si alloy and slag into a ladle, decarburizing the liquid Mn-Si alloy, and casting in a mould. And cooling the manganese-silicon alloy, crushing and packaging, and selling slag.
The manganese-silicon alloy composition is shown in Table 13, and the slag composition is shown in Table 14.
The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in Table 15.
TABLE 13 manganese silicon alloy composition Table
| Composition of the components | Mn | Si | C | P | S |
| Content% | 66.57 | 18.30 | 1.74 | 0.14 | 0.04 |
TABLE 14 slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | MnSi | MgO | Impurity(s) |
| Content (%) | 31.71 | 24.63 | 7.41 | 2.63 | 2.27 | 31.34 |
TABLE 15 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Mn | Fe |
| Content (%) | 18.67 | 12.32 | 43.10 | 4.05 | 1.60 | 10.27 | 8.10 | 1.89 |
Comparative example 2
A method for preparing manganese-silicon alloy from lithium ore and enriching lithium comprises the following specific steps:
other conditions were similar to example 2 except that the high carbon ferrochrome was changed to manganese ore, the composition of which was as follows: mn 34.4%, siO 2 15.69%，Fe 6.4%，Al 2 O 3 5%，CaO 9.07%，MgO 9%。
(1) Crushing lithium ore, manganese ore, a carbon reducing agent and a calcium additive, and then proportioning to obtain a mixture;
the specific proportioning is as follows: mixing according to the mass ratio of spodumene to C in semi-coke of 3:1 and the molar ratio of Si in spodumene to Mn in manganese ore of 2:1, wherein the mass of quicklime is 5% of the total mass of the other three materials (spodumene, semi-coke and manganese ore);
the granularity of the semi-coke is 25mm, the manganese ore is 30mm blocky, the spodumene is 20-100mm blocky, and the crushing treatment is not needed. Spodumene composition analysis is shown in table 5;
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1750 ℃, and smelting for 8 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce manganese-silicon alloy liquid and high-aluminum slag. And discharging the liquid Mn-Si alloy and slag into a ladle, decarburizing the liquid Mn-Si alloy, and casting in a mould. And cooling the manganese-silicon alloy, crushing and packaging, and selling slag.
The manganese-silicon alloy composition is shown in Table 16, and the slag composition is shown in Table 17.
The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in a table 18.
TABLE 16 manganese silicon alloy composition table
| Composition of the components | Mn | Si | C | P | S |
| Content% | 65.34 | 18.02 | 1.8 | 0.26 | 0.04 |
TABLE 17 slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | MnSi | MgO | Impurity(s) |
| Content (%) | 34.47 | 32.95 | 6.65 | 2.43 | 1.33 | 22.17 |
TABLE 18 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Mn | Fe |
| Content (%) | 22.01 | 30.95 | 30.11 | 4.21 | 4.29 | 4.55 | 2.54 | 1.34 |
Comparative example 3
A method for preparing manganese-silicon alloy from lithium ore and enriching lithium comprises the following specific steps:
other conditions were similar to example 3 except that the high carbon ferrochrome was changed to manganese ore, the composition of which was as follows: mn 34.4%, siO 2 15.69%，Fe 6.4%，Al 2 O 3 5%，CaO 9.07%，MgO 9%。
(1) Crushing lithium ore, manganese ore, a carbon reducing agent and a calcium additive, and then proportioning to obtain a mixture;
the specific proportioning is as follows: mixing according to the mass ratio of spodumene to C in semi-coke of 2.5:1 and the molar ratio of Si in spodumene to Mn in manganese ore of 2.5:1, wherein the mass of quicklime is 6% of the total mass of the other three materials (spodumene, semi-coke and manganese ore);
the granularity of the coke is 25mm, the manganese ore is 30mm blocky, the spodumene is 20-100mm blocky, and the crushing treatment is not needed. Spodumene composition analysis is shown in table 5;
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace, introducing nitrogen to raise the temperature of the submerged arc furnace to 1850 ℃, and smelting for 4 hours; the mixture undergoes deoxidization reduction reaction in a high-temperature furnace to finally produce manganese-silicon alloy liquid and high-aluminum slag. And discharging the liquid Mn-Si alloy and slag into a ladle, decarburizing the liquid Mn-Si alloy, and casting in a mould. And cooling the manganese-silicon alloy, crushing and packaging, and selling slag.
The manganese-silicon alloy composition is shown in Table 19, and the slag composition is shown in Table 20.
The flue gas of the submerged arc furnace passes through a flue arranged above, negative pressure induced draft is adopted, and a lithium mixture is collected in a flue gas recovery system, and the composition of the lithium mixture is shown in a table 21.
TABLE 19 manganese silicon alloy composition table
| Composition of the components | Mn | Si | C | P | S |
| Content% | 65.73 | 18.07 | 1.84 | 0.23 | 0.03 |
TABLE 20 slag composition table
| Composition of the components | Al 2 O 3 | CaO | SiC | MnSi | MgO | Impurity(s) |
| Content (%) | 30.20 | 18.13 | 10.20 | 2.98 | 10.34 | 28.05 |
TABLE 21 lithium mixture composition table
| Composition of the components | Li | C | O | N | Al | Si | Mn | Fe |
| Content (%) | 14.32 | 20.31 | 16.53 | 10.15 | 5.38 | 16.65 | 13.20 | 3.45 |
Comparing examples 1, 2, 3 with comparative examples 1, 2, 3, the following conclusions can be drawn:
chromium has a higher melting point and boiling point than manganese and iron, and smeltingThe high temperature is more favorable for destroying the structure of the lithium ore to lead Li to be reduced and volatilized, and meanwhile, the chromium metal has small high temperature burning loss and less smoke dust entering, and is more favorable for enriching Li. Chromium is easier to combine with silicon than iron, is favorable for reaction, and inhibits volatilization of SiO; the high-carbon ferrochrome contains about 10% of carbon, chromium does not need carbon reduction, and the dosage of a carbonaceous reducing agent is reduced; the high-carbon ferrochrome contains less impurities, belongs to the field of feeding of concentrate into a furnace, and has small slag quantity and single component; the slag phase in the production process is easy to adjust, the furnace condition is stable, and the operation and the control are convenient; al in slag 2 O 3 High content, and is favorable for subsequent recovery and production of high-purity Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The consumption of 1 ton of silicon-chromium alloy is more than twice that of silicon-manganese alloy, and the treatment capacity of the silicon-chromium alloy is larger; the high-carbon ferrochrome is used as an additive, C is used as a reducing agent, al-O-Si bonds in spodumene are more easily damaged, lithium is volatilized and enriched in smoke dust, volatilization of SiO and manganese is reduced, impurities such as carbon, silicon and metal oxides in the smoke dust are fewer, the grade of lithium is greatly improved, preparation of lithium salts such as lithium carbonate is more facilitated, the production cost of the lithium salts is reduced, and the reduction temperature difference between the chromium and silicon is shortened due to the fact that chromium is higher than the reduction temperature of manganese, and the lithium salts are more easily combined with silicon. The generated heat is larger than that of manganese, which is favorable for the reduction of C and Si; the manganese-silicon alloy belongs to slag smelting, and because the manganese ore contains impurities, the slag quantity is large, so that Al in the aluminum slag 2 O 3 The content is low; manganese ore itself contains SiO 2 15.69 percent, and other impurities are high in content, so that the dosage of the semi-coke is increased; mineral powder and carbon powder are easy to enter a flue and are mixed with Li ash in the production process; the content of Al and Si detected from the lithium-rich ash of the manganese-silicon alloy is higher than that of the silicon-chromium alloy, so that the loss of silicon and aluminum is proved, the content of Li in the lithium-rich ash is correspondingly reduced, and the cost for producing lithium salt by a subsequent wet method is increased.
The invention has been described with reference to the above-described related embodiments and drawings, however, the above-described embodiments are merely examples of practicing the invention. It should be noted that the disclosed embodiments do not limit the scope of the invention. On the contrary, modifications and equivalent arrangements included within the spirit and scope of the claims are intended to be included within the scope of the invention.
Claims (6)
1. A method for preparing a silicon-chromium alloy from lithium ore and enriching a lithium mixture, comprising the steps of:
(1) Mixing lithium ore, high-carbon ferrochrome, a carbon reducing agent and a calcium additive to obtain a mixture; the high-carbon ferrochrome comprises the following elements in percentage by mass: cr is more than or equal to 55%, fe is more than or equal to 30%, C is more than or equal to 6% and less than or equal to 10%;
(2) Adding the mixture obtained in the step (1) into a sealed submerged arc furnace for high-temperature reduction reaction, wherein the temperature of the high-temperature reduction reaction is 1000-2200 ℃, the reaction time is 1-24 h, smelting to obtain silicon-chromium alloy and blast-aluminum slag, and recovering the lithium mixture in a flue gas cooling system of the submerged arc furnace.
2. The method for preparing a silicon-chromium alloy and enriching a lithium mixture from lithium ore according to claim 1, wherein the lithium ore is one or more of spodumene, lepidolite and clay type lithium ore which are mixed in any proportion.
3. The method for preparing a silicon-chromium alloy and enriching a lithium mixture from lithium ore according to claim 1, wherein the high carbon ferrochrome is one or a mixture of a plurality of brands in GB/T5683-2008 in any proportion.
4. The method of preparing a silicon-chromium alloy and enriching a lithium mixture from a lithium ore according to claim 1, wherein the carbon reducing agent is one or a mixture of two of semi-coke and coke.
5. The method of preparing a silicon-chromium alloy and enriching a lithium mixture from a lithium ore according to claim 1, wherein the calcium additive is one or a mixture of two of quicklime or limestone.
6. The method for preparing a silicon-chromium alloy and enriching a lithium mixture from lithium ore according to claim 1, wherein the mass ratio of the lithium ore to the C in the carbon reducing agent in the mixture of step (1) is 1-5:1; the molar ratio of Si in the lithium ore to Cr in the high-carbon ferrochrome is 1-4:1; the addition amount of the calcium additive is 5-20% of the total mass of the lithium ore, the carbon reducer and the high-carbon ferrochrome.
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