CN101476049B - Method for removing magnesium from metallic ore - Google Patents
Method for removing magnesium from metallic ore Download PDFInfo
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- CN101476049B CN101476049B CN2009100940092A CN200910094009A CN101476049B CN 101476049 B CN101476049 B CN 101476049B CN 2009100940092 A CN2009100940092 A CN 2009100940092A CN 200910094009 A CN200910094009 A CN 200910094009A CN 101476049 B CN101476049 B CN 101476049B
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- magnesium
- metallic ore
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- reductive agent
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000011777 magnesium Substances 0.000 title abstract description 52
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title abstract description 46
- 229910052749 magnesium Inorganic materials 0.000 title abstract description 41
- 230000002829 reductive effect Effects 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 23
- 239000000395 magnesium oxide Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 10
- 239000011707 mineral Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000003245 coal Substances 0.000 claims description 7
- 239000000571 coke Substances 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000005188 flotation Methods 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000010953 base metal Substances 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- LWNCNSOPVUCKJL-UHFFFAOYSA-N [Mg].[P] Chemical compound [Mg].[P] LWNCNSOPVUCKJL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity 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
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to method of reducing magnesium from metallic ore by using carbon as the reductive. The method comprises steps of drying the metallic ore containing magnesium, mixing the dried metallic ore and the reductive in proportion and briquetting under a pressure of 15 Pa-50Pa and a temperature of 1400-1700 DEG C, reducing magnesium vapor from the foreign matters containing magnesium though a vacuum carbon thermoreduction process, condensing the magnesium vapor to form metal magnesium. Magnesium removing rate of metallic ore is bigger than 75% and purity of metal magnesium obtained through condensing is bigger than 95%.The invention has characteristics of simple process flow, convenient operations and raw materials with wide adaptability and in the process of reducing magnesium from metallic ore, well-crystallized metal magnesium can be obtained at the same time, the whole reaction process is performed in vacuum, therefore, the reaction has no pollution to environment.
Description
One, technical field
The present invention relates to a kind of from metallic ore the method for de-magging, belong to a kind of vacuum metallurgy method.
Two, technical background
Magnesium is one of the widest element of occurring in nature distribution, and it has very strong chemically reactive, all contains the compound of magnesium in many metallic ores of occurring in nature, as containing MgO10%-30% in the red soil nickel ore ore deposit, also contains the compound of small amount of magnesium in the vanadium titano-magnetite.These mineral can not be directly used in the production of MAGNESIUM METAL, and the production of other metals is had bigger influence or harm, and when carrying nickel as red soil nickel ore, the existence of MgO increases the vitriolic consumption greatly.Therefore in industrial production, handle and all can design special demagging operation when containing the magnesium addition metallic ore.In the industrial production there be the magnesium method that removes commonly used at present: (1) neutralization precipitation base metal demagging method; (2) concentrate pickling demagging method; (3) fluorochemical precipitation base metal demagging method; (4) condensing crystal demagging method; (5) efficient extraction agent separates base metal demagging method.Commonly usedly in hydrometallurgy remove magnesium method and can be divided into two classes: the one, when containing Mg amount 〉=0.6% when vulcanised ore concentrate, adopt dilute sulphuric acid washing method except that Mg, make Mg with MgSO
4Enter into washings and get rid of, this method can be removed the magnesium in the vulcanised ore concentrate effectively, but can produce a large amount of sal epsom when Mg content is high, has strengthened the burden of environment.Another kind of is solution to be put together cool off demagging.These processing methodes all can make magnesium content be controlled at lower level by control of process condition.But all should deposit mode and processing requirement and different according to the tax of magnesium addition in the concentrate.
All once technology for removal of magnesium from phosphorous had been done a large amount of research both at home and abroad since the eighties of last century, China patent 88105674.X discloses a kind of relevant technology for removal of magnesium from phosphorous ore.It is to use certain iron-holder, and 95% crosses 100 purpose ground phosphate rock, be made into the slurries of certain solid-to-liquid ratio with water, feeding contains the waste gas of sulfurous gas, pH value in the slurries is remained between 2.0～5.0, after reacting 8～24 hours at normal temperatures and pressures, analyse method etc. with sedimentation and filtration method or pen again, magniferous liquid phase is separated with the phosphorus concentrate, discharge after waste water is handled with appropriate means or use it for anything else, gained phosphorus concentrate can improve 1～7% grade, magnesium content is below 1%, and phosphorus decreases less than 5%, and this technology also has the effect of desulfurization, remarkable in economical benefits simultaneously.Patent 200710065792.0 also discloses a kind of method of demagging from phosphate ore.This method is to adopt the reverse flotation of static microbubble floatation column to remove magnesium method, and used flotation separation equipment is static microbubble floatation column.The phosphorus ore raw ore is after fragmentation, ore grinding and classification, in the mineralising groove, add reverse floatation agent and the abundant mixing of ore pulp, enter flotation in the static microbubble floatation column, size mixing and floatation process carry out simultaneously, ore pulp is after flotation, the gained foam is a flotation tailings mutually, and product is low magnesium phosphorus concentrate at the bottom of the post, can satisfy the Wet-process Phosphoric Acid Production requirement.
External researchist has also done a large amount of research to technology for removal of magnesium from phosphorous.United States Patent (USP) 09/351,956 (Methodfor removing magnesium from brine to yield lithium carbonate) discloses a kind of seawater that is used for and has produced the magnesium method that removes that the Quilonum Retard engineering uses; United States Patent (USP) 08/317,050 (Method for removing magnesiumfrom aluminum-magnesium alloys with engineered scavenger compound) discloses the method that a kind of compound of a kind of usefulness removes magnesium in the aluminium-magnesium alloy.
Three, summary of the invention
The objective of the invention is to: provide a kind of from metallic ore the method for de-magging, remove the method for magnesium addition in the ore deposit with vacuum carbothermal reduction, with carbon (coal or coke) is reductive agent, making impurity element magnesium in the ore deposit be reduced into magnesium vapor by the vacuum reducing process removes, can get well-crystallized's solid metal magnesium behind this vapour condensation, its purity is greater than 95%; The decreasing ratio of magnesium is greater than 75%.
The present invention finishes according to the following steps
(1) dried raw material and reductive agent are crushed to 100～300 orders respectively; Allocate coal or coke and mixing into for stoichiometric 2～20 times according to magnesium oxide mole in the reaction (a);
MgO(s)+C(s)＝CO(g)+Mg(g) (a)
(2) with mixing raw material with 5MPa～30MPa pressure briquetting, and carry out vacuum carbothermal reduction in the adding vacuum oven and react, open vacuum system, control furnace pressure less than 20Pa after, insulation reaction when being warming up to 550 ℃～700 ℃ with the temperature rise rate of 5 ℃/min～15 ℃/min, insulation finishes after pressure drops to less than 50Pa; And then insulation reaction when being warming up to 1400 ℃～1700 ℃ with the temperature rise rate of 5 ℃/min～15 ℃/min, drop to less than 50Pa to pressure, close heating system;
(3) behind temperature in the vacuum oven＜200 ℃, close vacuum system, be cooled to room temperature again, open vacuum oven, from reactor, obtain the metalliferous mineral behind the de-magging, obtain well-crystallized's metal MAG block simultaneously on the condenser.
Described feed metal ore deposit main component is: 8～35wt%MgO, 10～50wt%Fe
2O
3, 30～45wt%SiO
2: reductive agent is coal or coke;
Advantage of the present invention is can well collect to need not to add any other additive and fuel etc. in magnesium, the process when removing magnesium, and entire reaction course is carried out in a vacuum, and is environmentally friendly.The present invention compares with known technology, and its process object is for containing MgO or MgCO
3Metalliferous mineral, under vacuum condition, adopt carbothermic reduction to remove magnesium in the ore deposit, characteristics such as it is simple to have a technical process, and magnesium is removed and directly obtains MAGNESIUM METAL in the process, and is applied widely, environmentally friendly,
Four, embodiment
Embodiment 1: contain MgO 8.6%, 30wt%Fe
2O
3, 40wt%SiO
2Metallic ore 500g, the reductive agent coal or the coke that add 10 times of MgO mole chemical equivalents, briquetting under the 30MPa pressure, the vacuum oven of packing into is opened vacuum system, when pressure-stabilisation begins to heat up during at 20Pa, being warming up to 600 ℃ with the speed of 10 ℃/min is incubated, this moment, furnace pressure reached 68Pa, when treating that pressure drops to 43Pa, finished insulation; Then with the speed of 10 ℃/min be warming up to 1700 ℃ this moment furnace pressure be 196Pa, when furnace pressure is reduced to 40Pa, finish insulation, close heating system; After temperature in the stove is reduced to 180 ℃, close vacuum system and cooling water system; Treat that temperature is opened vacuum oven to normal temperature in the stove, the metalliferous mineral after the taking-up demagging, the decreasing ratio of magnesium is greater than 88%; By Mg content analyze Mg content (in magnesium oxide)＜0.5% in the metalliferous mineral after the demagging, and take off the metal of condensation from condenser, by X-ray diffraction analysis, be defined as MAGNESIUM METAL, its purity＞98%.
Embodiment 2: the metallic ore 500g that contains MgO 31.24wt%, the reductive agent coal or the coke that add 5 times of mole chemical equivalents, briquetting under the 20MPa pressure, the vacuum oven of packing into is opened vacuum system, when pressure-stabilisation begins to heat up during at 15Pa, being warming up to 550 ℃ with the speed of 5 ℃/min is incubated, this moment, furnace pressure reached 59Pa, when treating that pressure drops to 35Pa, finished this section insulation; Then with the speed of 5 ℃/min be warming up to 1500 ℃ this moment furnace pressure be 138Pa, when furnace pressure is reduced to 37Pa, finish insulation, close heating system; After temperature in the stove is reduced to 180 ℃, close vacuum system and cooling water system; Treat that temperature is opened vacuum oven to normal temperature in the stove, take out the metalliferous mineral after the demagging in the crucible, the decreasing ratio of magnesium is greater than 83%; By Mg content analyze Mg content (in magnesium oxide)＜1.9% in the metalliferous mineral after the demagging, and take off the metal of condensation from condenser, by X-ray diffraction analysis, be defined as MAGNESIUM METAL, its purity＞95%.
Embodiment 3: the metallic ore 500g that contains MgO 15.67%, the reductive agent coal or the coke that add 2.5 times of mole chemical equivalents, briquetting under the 5MPa pressure, the vacuum oven of packing into is opened vacuum system, when pressure-stabilisation begins to heat up during at 8Pa, being warming up to 700 ℃ with the speed of 15 ℃/min is incubated, this moment, furnace pressure reached 76Pa, when treating that pressure drops to 40Pa, finished insulation; Then with the speed of 15 ℃/min be warming up to 1400 ℃ this moment furnace pressure be 128Pa, when furnace pressure is reduced to 43Pa, finish insulation, close heating system; After temperature in the stove is reduced to 200 ℃, close vacuum system and cooling water system; Treat that temperature is opened vacuum oven to normal temperature in the stove, take out the metalliferous mineral after the demagging, by Mg content analyze Mg content (in magnesium oxide)＜2.1% in the metalliferous mineral after the demagging, the decreasing ratio of magnesium is greater than 76%; And take off the metal of condensation from condenser, by X-ray diffraction analysis, be defined as MAGNESIUM METAL, its purity＞96%.
Claims (1)
1. the method for a de-magging from metallic ore, it is feature: it is finished according to the following steps,
(1) will be crushed to 100～300 orders respectively with reductive agent after the drying of feed metal ore deposit, allocate reductive agent and mixing into for stoichiometric 2～20 times according to the mole of magnesium oxide in the feed metal ore deposit and reductive agent reaction; Described feed metal ore deposit is main component 8～35wt%MgO, 10～50wt%Fe
2O
3, 30～45wt%SiO
2The magnesium oxide ore deposit; Described reductive agent is coal or coke;
(2) with mixing raw material with briquetting under 5MPa～30MPa pressure, and carry out vacuum carbothermal reduction in the adding vacuum oven and react, open vacuum system, control furnace pressure less than 20Pa after, insulation when being warming up to 550 ℃～700 ℃ with the temperature rise rate of 5 ℃/min～15 ℃/min, insulation reaction when continuing temperature rise rate with 5 ℃/min～15 ℃/min being warming up to 1400 ℃～1700 ℃ after pressure drops to less than 50Pa drops to less than 50Pa to pressure, closes heating system;
(3) behind temperature in the vacuum oven＜200 ℃, close vacuum system, be cooled to room temperature again, open vacuum oven, from reactor, obtain the metalliferous mineral behind the de-magging, obtain crystal type metal MAG block on the condenser simultaneously.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100940092A CN101476049B (en) | 2009-01-05 | 2009-01-05 | Method for removing magnesium from metallic ore |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100940092A CN101476049B (en) | 2009-01-05 | 2009-01-05 | Method for removing magnesium from metallic ore |
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| CN101476049A CN101476049A (en) | 2009-07-08 |
| CN101476049B true CN101476049B (en) | 2010-06-09 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589878B (en) * | 2013-11-07 | 2015-03-11 | 昆明理工大学 | Method for removing magnesium from calcium-containing material |
| TWI594954B (en) * | 2014-12-12 | 2017-08-11 | Taiwan Carbon Nano Tech Corp | A method of producing electrical energy from a metal electrode made from seawater |
| CN106191467A (en) * | 2016-07-12 | 2016-12-07 | 吉林市润成膜科技有限公司 | A kind of method that former Smelting magnesium prepares porous silicon simultaneously |
| AU2022390038A1 (en) * | 2021-11-16 | 2024-04-11 | Big Blue Technologies, Inc. | A method for continuous production of magnesium metal by metallothermic reduction of magnesium bearing ore and condensation of liquid magnesium |
| CN114737057B (en) * | 2022-03-24 | 2024-03-26 | 东北大学 | Method for preparing high vapor pressure metal by carbothermal reduction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035093A (en) * | 1988-02-13 | 1989-08-30 | 湖南大学 | A kind of technology for removal of magnesium from phosphorous ore |
| US6143260A (en) * | 1998-07-16 | 2000-11-07 | Chemetall Foote Corporation | Method for removing magnesium from brine to yield lithium carbonate |
| CN101049584A (en) * | 2007-04-09 | 2007-10-10 | 云南省化工研究院 | Method for demagging from phosphate ore |
-
2009
- 2009-01-05 CN CN2009100940092A patent/CN101476049B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035093A (en) * | 1988-02-13 | 1989-08-30 | 湖南大学 | A kind of technology for removal of magnesium from phosphorous ore |
| US6143260A (en) * | 1998-07-16 | 2000-11-07 | Chemetall Foote Corporation | Method for removing magnesium from brine to yield lithium carbonate |
| CN101049584A (en) * | 2007-04-09 | 2007-10-10 | 云南省化工研究院 | Method for demagging from phosphate ore |
Non-Patent Citations (4)
| Title |
|---|
| 胡显智，张文彬.云南某铂钯矿酸浸除镁及浸出液综合利用研究.矿产综合利用 2.2003,(2),3-8. |
| 胡显智,张文彬.云南某铂钯矿酸浸除镁及浸出液综合利用研究.矿产综合利用 2.2003,(2),3-8. * |
| 陆建刚.磷矿除镁新工艺.硫磷设计与粉体工程 3.1994,(3),43-44. |
| 陆建刚.磷矿除镁新工艺.硫磷设计与粉体工程 3.1994,(3),43-44. * |
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