CN101338365B - Synthesizing method for molybdenum-nickel ore - Google Patents
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- CN101338365B CN101338365B CN2008100683826A CN200810068382A CN101338365B CN 101338365 B CN101338365 B CN 101338365B CN 2008100683826 A CN2008100683826 A CN 2008100683826A CN 200810068382 A CN200810068382 A CN 200810068382A CN 101338365 B CN101338365 B CN 101338365B
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Abstract
The invention discloses a method for comprehensively processing a molybdenum-nickel ore which needs to solve the technical problem of achieving the high extraction rate of molybdenum, nickel, zinc, copper and lead as well as comprehensively utilizing the valuable component of a carbon molybdenum-nickel ore. The invention includes the following steps: grinding a raw ore material to 100 to 400 meshes; pre-extraction, terminal-extraction, the processing of the slag of terminal-extraction and the separation of a pre-extraction liquid. Compared with the prior art, the invention has a high comprehensive recycling rate; the molybdenum-nickel achieves 99 percent; the other nonferrous metals achieve 96 percents. Besides, the method of the invention avoids the valuable component from being lost during the next separation process; the pre-extraction liquid is closed and circulated during the technique; the waste water drain is removed; the demand of the technique to a device is low; the used chemical materials are cheap; the technical condition is gentle; the cost is low; the hidden safety danger brought by the traditional high temperature and high pressure operation is removed; the production process is easy to realize mechanization.
Description
Technical field
The present invention relates to a kind of extracting method of non-ferrous metal molybdenum nickel, the extraction in particularly a kind of carbon molybdenum nickel ore deposit is handled and the comprehensive method that reclaims.
Background technology
The carbon molybdenum nickel ore deposit belongs to the complicated Mineral resources of multiple metal level, and the molybdenum grade is at 2-8%, form tax with sulphur molybdenum ore and molybdenum glance is stored in the cryptocrystalline colloidal state sulfide, the molybdenum grade is below 3%, and kenel is millerite, vaesite, niccolite, and valuable constituent such as association copper-lead zinc-silver.In this ore deposit iron 15-20% is arranged still in addition, aluminium 1-5%, sulphur 20-30%, recyclable compositions such as charcoal 5-15%, but select the smelting difficulty big, the comprehensive difficulty that reclaims.Prior art does not still have very perfect way to the processing of above-mentioned molybdenum nickel minerals, the technology of obtaining molybdenum nickel at above-mentioned ore deposit mainly contains: Chinese patent application CN88102597.6 disclosed method, adopt earlier ore materials desulfurization with roasting technique under the 30-570 degree, again with vitriol oil heating thermalization 2-3 hour, its post-heating leaches, immersion liquid is fallen acidity with the precipitation molybdenum with ammoniacal liquor, and mother liquor extracts deironing, raffinate reclaim(ed) sulfuric acid nickel ammonium behind the extraction molybdenum earlier again.The advantage of this method is: technology is simply direct, and shortcoming is: have a large amount of SO
2Pollute, and be difficult to take into account between the consumption of acid and ammonia and the leaching yield.Chinese patent application CN2006100331788.8 disclosed method proposes under a kind of highly basic heating condition, and with the method that dioxygen oxidation leaches, its advantage is: exempted SO
2Pollution, processing unit is simple, it is low that subsidiary material consume, shortcoming is: leaching yield is low, and the unexposed further separation method of purifying.Chinese patent application CN99114737.5 and CN99114736.7 disclosed method have proposed respectively in diluted acid and weak base medium, and with the method that oxygenant leaches, leach liquor is through extracting and separating molybdenum and nickel, but do not propose concrete oxygenant and purification scheme.
Summary of the invention
The method that the purpose of this invention is to provide the comprehensive treating process of a kind of molybdenum nickel minerals, the technical problem that solve are to reach molybdenum nickel zinc-copper lead high leaching yield is arranged, the valuable constituent in comprehensive utilization carbon molybdenum nickel ore deposit.
The present invention is by the following technical solutions: the method for a kind of molybdenum nickel minerals comprehensive treating process may further comprise the steps:
One, carbon molybdenum nickel green ore material is ground to the 100-400 order; Two, with whole immersion liquid the raw ore material after grinding is carried out preimpregnation, the gained solid phase is the preimpregnation slag, the processing condition of preimpregnation are: raw ore material and whole immersion liquid mass ratio=1: 5-10, temperature: 90-120 degree, pressure: 0-2 normal atmosphere, time 30-120 minute, whole immersion liquid composition was: molybdenum 5-25g/l, nickel 3-25g/l, chlorine 50-300g/l; Three, the preimpregnation slag soaks eventually and obtains soaking eventually slag, the quality solid-to-liquid ratio of preimpregnation slag and immersion liquid is 6-12, feed chlorine, the processing condition of soaking eventually are: iron concentration 1-8M, temperature 85-150 degree, pressure 0-5 normal atmosphere, time 30-7200 minute, it is that the mother liquor of 10-30% is as immersion liquid that tail washings adds mass ratio, tail washings composition: ammonium chloride 1-10g/l, ammonium sulfate 1-10g/l and be lower than sodium, potassium, iron and the aluminium of 50g/l, be lower than copper, lead, zinc, molybdenum and the nickel of 1g/l, mother liquor composition: iron 20-125g/l, chlorine 45-300g/l, ammonia radical ion 1-20g/l; Four, soak slag eventually and ammoniacal liquor quality solid-to-liquid ratio is 1-0.1, at room temperature stirred 1 hour pH 〉=10, and obtaining liquid phase after the centrifugation is the ammonia wash water; Five, the ammonia wash water feeds steam heating ammonia still process, steams mother liquor behind the ammonia in the crystallizer tank crystallisation by cooling, and crystallization is the ammonium tetramolybdate product.
The carbon molybdenum nickel green ore material of the inventive method is ground to 320 orders.
Soak the end of the inventive method and adopt three sections segmentations to carry out.
Soak slag and ammoniacal liquor the end of the inventive method and stir, the solid phase after the centrifugation is the ammonia washery slag, compression moulding after 80-150 ℃ kerosene is washed sulphur, and burning gained ash content enters the precious metal recycle section and handles, and reclaims palladium, platinum noble metals.
The preimpregnation gained liquid phase of the inventive method is a presoak, and with sulphur hydrogenation ammonium precipitated copper, silver, lead, zinc, the pH that adjusts the sulfide precipitation process with ammoniacal liquor is 3.
The liquid phase of the sulphur hydrogenation ammonium post precipitation of the inventive method, the solid that produces behind vaporizer dissolves and boils through hydrochloric acid and hydrogen peroxide again, through anion-exchange column, molybdenum is attracted on the post, and with ammoniacal liquor desorb molybdenum, evaporative crystallization is the ammonium tetramolybdate product after the magnesium chloride dephosphorization.
The surplus liquid of exchange after the anion-exchange column of the inventive method is used further vulcanizes to pH=6 with ammonia-sulphur hydrogenation ammonium, and the gained throw out is controlled pH=11 with sodium hydroxide NaOH neutralization, separates through whizzer, and precipitation slag obtains crystalline sulfuric acid nickel product through sulfuric acid dissolution.
The liquid phase that the throw out of the inventive method separate to produce through whizzer is filtered the oven dry of gained throw out and is aluminium hydroxide with the sulfuric acid neutrality that neutralizes, and becomes the aluminium sesquioxide product through roasting.
The surplus liquid of exchange after the anion-exchange column of the inventive method is used, further vulcanize to pH=6 with ammonia-sulphur hydrogenation ammonium, gained sulfuration mother liquor, pack in enamel pot or the stainless cylinder of steel, under the condition of 80-200 ℃ heating, blast air, air pressure 0-2MPa, regulating pH with ammonia is 0-3, leach the pin scum after roasting obtain the ferric oxide product.
The liquid phase that the throw out of the inventive method separate to produce through whizzer is filtered the mother liquor of gained and is arranged into circulation fluid deposit pond with the sulfuric acid neutrality that neutralizes; The surplus liquid of exchange after described anion-exchange column is used, further vulcanize to pH=6 with ammonia-sulphur hydrogenation ammonium, gained sulfuration mother liquor, pack in enamel pot or the stainless cylinder of steel, under the condition of 80-200 ℃ heating, blast air, air pressure 0-2MPa, regulating pH with ammonia is 0-3, the mother liquor that leaches behind the pin scum is removed sulfate radical with bariumchloride or barium sulphide, and ammonium chloride is removed in cooling again, enters circulation fluid deposit pond.
The present invention compared with prior art, the comprehensive recovery height, molybdenum nickel leaching yield reaches 99%, other non-ferrous metals reach 96%, avoid valuable constituent to run off in sepn process subsequently, presoak is closed circulation in technology, eliminates discharge of wastewater, technology to equipment require low, used industrial chemicals cheapness, the processing condition gentleness, cost is low, eliminated the potential safety hazard that the conventional high-temperature high top pressure operation brings, production process is easy to realize mechanize.
Description of drawings
Fig. 1 is the FB(flow block) of the embodiment of the invention.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.As shown in Figure 1, operational path S represents solid phase, and L represents liquid phase, and G represents gas phase.The method of molybdenum nickel minerals of the present invention comprehensive treating process, for handling the technology in carbon molybdenum nickel ore deposit, comprise three process sections: the leaching of raw ore separates with the processing of soaking slag, presoak.
One, the leaching of raw ore may further comprise the steps:
1, the raw ore material is ground to the 100-400 order, is preferably 320 orders;
2, with whole immersion liquid proportion d is 1.0-1.2, the pit wood material is carried out preimpregnation, whole immersion liquid composition is: molybdenum 525g/l, nickel 3-25g/l, chlorine 50-300g/l, the processing condition of preimpregnation are: raw ore material behind the mill and whole immersion liquid mass ratio=1: 5-10, temperature: 90-120 degree, pressure: 0-2 normal atmosphere, time 30-120 minute, it is purpose that preimpregnation is converted into ferrous with iron, the over-drastic preimpregnation is deleterious, preimpregnation gained solid phase is the preimpregnation slag, the preimpregnation slag ingredient is near raw ore, and only the ferronickel sulphur content decreases, and the gained liquid phase is a presoak, proportion d is 1.0-1.2, and the presoak composition is: molybdenum 5-25g/l, nickel 3-25g/l, iron 25-125g/l, chlorine 50-300g/l, copper 0.1-50g/l, zinc 10g/l.
3, soak the end of preimpregnation slag, use the tail washings of the centrifugal station that extracts from circulation fluid deposit pond, add mass ratio and be mother liquor behind the heavy nickel of 10-30% as leach liquor, tail washings composition: ammonium chloride NH
4CLl 1-10g/l, ammonium sulfate (NH
4)
2SO
41-10g/l and be lower than sodium, potassium, iron and the aluminium of 50g/l is lower than copper, lead, zinc, molybdenum and the nickel of 1g/l, mother liquor composition: iron 20-125g/l, chlorine 45-300g/l, ammonia radical ion NH
4+ 1-20g/l, the quality solid-to-liquid ratio that preimpregnation slag and tail washings add behind the mother liquor is 6-12, feeding chlorine carries out soaking end, the flow of chlorine is by the consumption of solution to chlorine, automatically replenish by pressure equilibrium, soak eventually and be lower than thousandth with the molybdenum ambrose alloy zinc content in the slag and get final product, soak the leaching of employing one workshop section or multiplex's section eventually, it is to make solid one by one with liquid gas hybrid reaction that multiplex's section leaches, and leaches more completely and lower raw materials consumption to reach.The processing condition of soaking eventually are: iron concentration 1-8M, temperature 85-150 degree, pressure 0-5 normal atmosphere, time 30-7200 minute, the equal content of molybdenum, nickel, copper and zinc that soaks eventually in the slag of back is lower than thousandth, thereby make leaching yield enough high, leaching process has the chloride discharge of intermittent minute quantity, must handle emptying by the packing tower through being filled with Wingdale.Soaking the gained liquid phase eventually is whole immersion liquid, and the gained solid phase is for soaking slag eventually, and whole immersion liquid composition is: molybdenum 5-25g/l, nickel 3-25g/l, chlorine 50-300g/l, the composition that soaks slag eventually is: molybdenum 0.5-15g/l, sulphur 1-30g/l, charcoal 15-35g/l, gangue 25-75g/l.
Two, soak the processing of slag eventually, may further comprise the steps:
Earlier wash molybdenum through ammoniacal liquor with soaking slag end, at room temperature stirred 1 hour, the quality solid-to-liquid ratio is 1-0.1.The concrete processing method of dividing workshop section's washing that adopts: first section, soak slag eventually and adopt the segmentation agitator treating, the gained solid phase is one section washery slag after centrifugation, liquid phase is one section ammonia wash water; Second section, one section washery slag separates through two sections wash water washings, and solid phase is two sections washery slags, and liquid phase is two sections ammonia wash waters; The 3rd section, two sections washery slags are through ammonia absorption section gained weak ammonia agitator treating, and additional ammonia makes pH 〉=10.Solid phase after the separation is the ammonia washery slag, liquid phase is three sections ammonia wash waters, ammonia washery slag mass component is: sulphur 1-30%, charcoal 15-40%, gangue 30-80%, fuel is made in compression moulding after 80-150 ℃ kerosene is washed sulphur again, the surplus residue of burning is a white powder, does not contain harmful ingredients, and can be used as cement raw material, the gained ash content enters the precious metal recycle section and handles, and reclaims palladium, platinum noble metals.
The ammonia wash water feeds steam heating ammonia still process in evaporating pot, steam the crystallization that the mother liquor behind the ammonia leaches in crystallizer tank crystallisation by cooling, whizzer, be the ammonium tetramolybdate product, remaining mother liquor is used to absorb the ammonia that this section steams after molybdenum is taken off in ion-exchange, become weak ammonia, the ammonia that is used for next round is washed; The deep fat washing lotion of kerosene is through water cooling, slough after the crystallization sulphur after filtration, and the deep fat that is used for next round is washed.
Three, the separation of presoak may further comprise the steps:
1. the presoak of preimpregnation earlier steams thing sulphur hydrogenation ammonium with next step vaporizer generation, then use raw material sulphur hydrogenation ammonia during operation just, then necessarily replenish in the technological process according to the required work of precipitation, sulfide precipitation copper, silver, plumbous, zinc, adjust the terminal point pH to 3 of sulfide precipitation with ammoniacal liquor, precipitation adopts segmentation to wash with sulphur hydrogenation ammonium, washery slag is intermediates: copper, silver, plumbous, zinc powder, segmentation is washed the wash water of back sulphur hydrogenation ammonium through the vaporizer evaporate to dryness, the sulphur hydrogenation ammonium gas that evaporates is used for the sulfuration of previous step leach liquor, and the solid that produces in the vaporizer is through hydrochloric acid and hydrogen peroxide dissolving and boil the remaining oxygenant (H of destruction
2O
2) after, incorporate the mother liquor of aforementioned sulfide precipitation gained into, through anion-exchange column, molybdenum is attracted on the post, and iron, nickel, aluminium, ammonium are still in handing over surplus liquid.
2. negative molybdenum column-programming ammoniacal liquor segmentation desorb, evaporative crystallization produces ammonium tetramolybdate after the magnesium chloride dephosphorization, and mother liquor then is used to absorb the gas that evaporation produces, and is replenishing the desorb that is used for taking turns behind the ammonia.
3. the surplus liquid of exchange after anion-exchange column is used, further vulcanize to pH=5-6 with ammonia-sulphur hydrogenation ammonium, be preferably 6, separate through whizzer. the mother liquid obtained sulfuration mother liquor that is, be used for step processing down, the throw out of gained is controlled pH=11 with sodium hydroxide NaOH neutralization, and precipitation slag obtains crystalline sulfuric acid nickel product through sulfuric acid dissolution; The gas that produces absorbs producing sulphur hydrogenation ammonium with ammoniacal liquor, and alkali cleaning water filter the oven dry of gained precipitation and be aluminium hydroxide, but roasting becomes aluminium sesquioxide with the sulfuric acid neutrality that neutralizes, and the mother liquor that leaches aluminium hydroxide arranges that into circulation fluid deposit pond is standby.
4. with the sulfuration mother liquor after ammonia-sulphur hydrogenation ammonium sulfuration,-part is for soaking used the end that raw ore leaches step, surplus person packs in enamel pot or the stainless cylinder of steel, under the condition of 80-200 ℃ heating, blast the atmospheric oxidation precipitated iron, air pressure 0-2MPa, regulating pH with ammonia is 0-3, leaches the roasting of pin scum and obtains ferric oxide; The female slag of deferrization produces crystallization through filtering below 10 ℃, and the crystallization that leaches is the miscellany of ammonium chloride and ammonium sulfate, can be used as fertilizer.The deferrization mother liquor is removed sulfate radical with bariumchloride or barium sulphide, and ammonium chloride is removed in cooling again, enters circulation fluid deposit pond.
Method of the present invention centers on four parts: 1, molybdenum and nickel obtains, leaching yield surpasses 99%, 2, palladium, platinum, and the recovery of other precious metals, 3, the collection of valuable constituent aluminium, sulphur, charcoal and gangue, 4, the recovery of process chemistry liquid is recycled in the whole technological process.The collection effciency height of molybdenum and nickel, and can collect valuable constituent aluminium, sulphur, charcoal and gangue simultaneously, chemical liquid is recyclable, recycle, and cost is low.
Claims (7)
1. the method for molybdenum nickel minerals comprehensive treating process, may further comprise the steps: one, carbon molybdenum nickel green ore material is ground to the 100-400 order; Two, with whole immersion liquid the raw ore material after grinding is carried out preimpregnation, the gained solid phase is the preimpregnation slag, the processing condition of preimpregnation are: raw ore material and whole immersion liquid mass ratio=1: 5-10, temperature: 90-120 degree, pressure: 0-2 normal atmosphere, time 30-120 minute, whole immersion liquid composition was: molybdenum 5-25g/l, nickel 3-25g/l, chlorine 50-300g/l; Three, the preimpregnation slag soaks eventually and obtains soaking eventually slag, the quality solid-to-liquid ratio of preimpregnation slag and immersion liquid is 6-12, feed chlorine, the processing condition of soaking eventually are: iron concentration 1-8M, temperature 85-150 degree, pressure 0-5 normal atmosphere, time 30-7200 minute, it is that the mother liquor of 10-30% is as immersion liquid that tail washings adds mass ratio, tail washings composition: ammonium chloride 1-10g/l, ammonium sulfate 1-10g/l and be lower than sodium, potassium, iron and the aluminium of 50g/l, be lower than copper, lead, zinc, molybdenum and the nickel of 1g/l, mother liquor composition: iron 20-125g/l, chlorine 45-300g/l, ammonia radical ion 1-20g/l; Four, soak slag eventually and ammoniacal liquor quality solid-to-liquid ratio is 1-0.1, at room temperature stirred 1 hour pH 〉=10, and obtaining liquid phase after the centrifugation is the ammonia wash water; Five, the ammonia wash water feeds steam heating ammonia still process, steams mother liquor behind the ammonia in the crystallizer tank crystallisation by cooling, and crystallization is the ammonium tetramolybdate product; Described preimpregnation gained liquid phase is a presoak, with sulphur hydrogenation ammonium precipitated copper, silver, plumbous, zinc, the pH that adjusts the sulfide precipitation process with ammoniacal liquor is 3, the liquid phase of described sulphur hydrogenation ammonium post precipitation, the solid that behind vaporizer, produces, dissolve and boil through hydrochloric acid and hydrogen peroxide again, through anion-exchange column, molybdenum is attracted on the post, with ammoniacal liquor desorb molybdenum, evaporative crystallization is the ammonium tetramolybdate product after the magnesium chloride dephosphorization, and the surplus liquid of exchange after described anion-exchange column is used further vulcanizes to pH=6 with ammonia-sulphur hydrogenation ammonium, the gained throw out neutralizes with sodium hydroxide NaOH, control pH=11 separates through whizzer, and precipitation slag obtains crystalline sulfuric acid nickel product through sulfuric acid dissolution.
2. the method for molybdenum nickel minerals according to claim 1 comprehensive treating process is characterized in that: described carbon molybdenum nickel green ore material is ground to 320 orders.
3. the method for molybdenum nickel minerals according to claim 2 comprehensive treating process is characterized in that: soak described end and adopt three sections segmentations to carry out.
4. the method for molybdenum nickel minerals according to claim 3 comprehensive treating process, it is characterized in that: soak slag and ammoniacal liquor described end and stir, solid phase after the centrifugation is the ammonia washery slag, compression moulding after 80-150 ℃ kerosene is washed sulphur, burning gained ash content enters the precious metal recycle section and handles, and reclaims palladium, platinum noble metals.
5. the method for molybdenum nickel minerals according to claim 1 comprehensive treating process is characterized in that: the liquid phase that described throw out separate to produce through whizzer is filtered the oven dry of gained throw out and is aluminium hydroxide with the sulfuric acid neutrality that neutralizes, and becomes the aluminium sesquioxide product through roasting.
6. the method for molybdenum nickel minerals according to claim 1 comprehensive treating process, it is characterized in that: the surplus liquid of exchange after described anion-exchange column is used, further vulcanize to pH=6 with ammonia-sulphur hydrogenation ammonium, gained sulfuration mother liquor, pack in enamel pot or the stainless cylinder of steel, under the condition of 80-200 ℃ heating, blast air, air pressure 0-2MPa, regulating pH with ammonia is 0-3, leach the pin scum after roasting obtain the ferric oxide product.
7. the method for molybdenum nickel minerals according to claim 5 comprehensive treating process is characterized in that: the liquid phase that described throw out separate to produce through whizzer is filtered the mother liquor of gained and is arranged into circulation fluid deposit pond with the sulfuric acid neutrality that neutralizes; The surplus liquid of exchange after described anion-exchange column is used, further vulcanize to pH=6 with ammonia-sulphur hydrogenation ammonium, gained sulfuration mother liquor, pack in enamel pot or the stainless cylinder of steel, under the condition of 80-200 ℃ heating, blast air, air pressure 0-2MPa, regulating pH with ammonia is 0-3, the mother liquor that leaches behind the pin scum is removed sulfate radical with bariumchloride or barium sulphide, and ammonium chloride is removed in cooling again, enters circulation fluid deposit pond.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI511938B (en) * | 2014-07-09 | 2015-12-11 | Plummonix Industry Co Ltd | Reuse of Light - Containing Molybdenum Etching Waste |
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| CN102676803B (en) * | 2012-06-05 | 2013-07-17 | 南京元泰环保科技有限公司 | Resource utilization method for catalytic oxidation leaching of molybdenum and nickel from molybdenum-nickel ore |
| CN103290213A (en) * | 2013-05-21 | 2013-09-11 | 胡雷 | Process for recycling valuable metal from nickel laterite ores and simultaneously by-producing anhydrous calcium chloride |
| CN103509955B (en) * | 2013-07-17 | 2016-01-20 | 中信大锰矿业有限责任公司 | The technique of two ore deposit integrated process process red soil nickel ores and pyrolusite |
| CN105838882B (en) * | 2016-06-21 | 2017-11-17 | 昆明冶金研究院 | Separating molybdenum from nickel recovery process in a kind of nickel-molybdenum symbiotic ore oxygen pressure acid steep |
| CN107217135B (en) * | 2017-06-13 | 2018-10-19 | 山东国大黄金股份有限公司 | A kind of method of cyanidation gold-extracted waste slag multistage Concentration of Gold Ag-Cu-Zn and synthetical recovery |
| CN111411237A (en) * | 2020-04-29 | 2020-07-14 | 核工业北京化工冶金研究院 | Method for extracting and separating molybdenum in phosphorus-containing sulfuric acid system |
| CN113380558A (en) * | 2021-06-21 | 2021-09-10 | 贵州化工建设有限责任公司 | Slag pretreatment method and preparation method of supercapacitor electrode material |
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| TWI511938B (en) * | 2014-07-09 | 2015-12-11 | Plummonix Industry Co Ltd | Reuse of Light - Containing Molybdenum Etching Waste |
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