CN104745812A - Molybdenum-sulfur separation method - Google Patents
Molybdenum-sulfur separation method Download PDFInfo
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- CN104745812A CN104745812A CN201510138897.9A CN201510138897A CN104745812A CN 104745812 A CN104745812 A CN 104745812A CN 201510138897 A CN201510138897 A CN 201510138897A CN 104745812 A CN104745812 A CN 104745812A
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- molybdenum
- molybdenite concentrate
- pressure
- sulfur
- sulphur content
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Abstract
The invention discloses a molybdenum-sulfur separation method which comprises the following steps: after carrying out ball milling on the raw material molybdenite concentrate, putting in a high-pressure autoclave, adding a sulfuric acid solution according to the solid-liquid volume ratio of 4-10 times, and introducing oxygen to react at 160-240 DEG C under the pressure of 1.6-3.0 MPa for 8-16 hours, thereby implementing the molybdenum-sulfur separation. The method overcomes the defects of low environment friendliness, high reagent consumption, high production cost and unthorough separation in the existing molybdenum-sulfur separation method for molybdenite concentrate. The method uses the molybdenite concentrate containing 45-55% of molybdenum and 30-40% of sulfur as the raw material and adopts the dilute sulfuric acid solution to perform low-pressure oxygen leaching on the molybdenite concentrate, thereby achieving the goal of molybdenum-sulfur separation and providing beneficial conditions for the subsequent molybdenum-sulfur recovery step.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of molybdenum sulphur content from method.
Background technology
Molybdenum is mainly used in Iron And Steel Industry, as the additive of steel, is the important alloying element producing steel alloy, stainless steel and cast alloy iron.It can improve hardness and toughness, the creep-resistant property of steel.Add molybdenum in iron and can make pig-iron alloys, iron grain refining can be made, thus improve its high temperature, wear-resisting and acid resistance.The compound of molybdenum alloy and molybdenum is widely used in a lot of fields of modern technologies.
Known molybdenite concentrate realize molybdenum sulphur content from method be: 1) oxidizing roasting method: the object of roasting is that the molybdenum sulphur content of molybdenumdisulphide in molybdenite concentrate is left, and makes molybdenumdisulphide be converted into molybdic oxide after roasting.2) adding assistant oxidizing roasting method: in order to solve traditional sinter process generate flue gas in low concentration SO
2the problem easily polluted, adds various auxiliary agent as sodium carbonate, white lime, soft violent ore deposit etc. when molybdenite concentrate roasting, these auxiliary agents are directly the SO that roasting generates
2fixing, thus avoid it to enter flue gas.3) melting salt oxidation method: molybdenite concentrate is dissolved in Na
2cO
3-Na
2moO
4-Na
2sO
4and Na
2moO
4-Na
2sO
4fused-salt medium in, in fused salt, blast air, molybdenum generate Sodium orthomolybdate, the oxidized rear generation sodium sulfate of sulphur or SO
2.4) smelting bath smelting process: can moly-sulfide be dissolved based on matte, and not dissolve in concentrated molybdenum ore the gangue contents such as oxide compound, make moly-sulfide be dissolved in matte, matte carries out oxidation blowing again, makes moly-sulfide be oxidized into molybdenum oxide and be separated with matte.Matte is not oxidized, and it returns as utilization again.5) decomposition of nitric acid: adopt concentration of nitric acid 25% ~ 50%, Heating temperature is under the condition of more than 80 DEG C, can effectively by molybdenite concentrate oxidation generation precipitate molybdic acid, thus realize molybdenum sulphur content from.6) microbiological oxidation lixiviation process: adopt the bacterium of resistant to elevated temperatures thiophilic resistance to molybdenum ion by molybdenum leach realize sulphur content from method.Known molybdenite concentrate realize molybdenum sulphur content from method in table 1.
The known molybdenite concentrate of table 1 realize molybdenum sulphur content from method relative merits
sequence number | processing method | advantage | shortcoming |
1 | oxidizing roasting method | technique is simple, is beneficial to control. | but this technique produces a large amount of low concentration SO 2, environmental pollution is serious; Metal recovery rate is low, cost is high, the quality dissatisfaction of product, labour intensity large, associated metal comprehensive reutilization difficulty is large. |
2 | adding assistant oxidizing roasting method | low concentration SO in the flue gas of traditional sinter process generation can be solved 2the problem easily polluted. | although but auxiliary agent can avoid SO substantially 2gas purging, but the amount of reagent added is large, and the product of generation is as Na 2sO 4and CaSO 4be worth not high, production cost is higher. |
3 | melting salt oxidation method | speed of response quickly | the Na that the method generates 2moO 4na after water logging 2cO 3and Na 2sO 4be dissolved into therewith in water, these three kinds of compounds solubleness in water is all higher, is difficult to realize effective separation |
4 | smelting bath smelting process | technique is simple. | in molybdenite concentrate, pyrite sulfides etc. are dissolved in matte, cause matte to be oxidized FeS sulfides impurity when blowing and enter into molybdenum oxide, cause difficulty to subsequent technique. |
5 | decomposition of nitric acid | decrease oxidizing roasting operation, avoid low concentration SO 2pollution. | consume a large amount of nitric acid, concentrate requires that granularity wants thin, and equipment palpus erosion resistance, cost is higher. |
6 | microbiological oxidation lixiviation process | technique is simple, easy to operate, energy consumption is low, pollution-free. | leaching yield is low, and length consuming time, cost is high. |
Disclose molybdenum nickel minerals under dilute sulphuric acid environment in the document technique of pressure leaching molybdenum and nickel " from the molybdenum nickel minerals ", can in molybdenum nickel minerals-divalent S is direct oxidation into+6 valencys, S thus generate SO
4 2-, avoid low concentration SO
2the discharge of tail gas; + 4 valency Mo can be direct oxidation into+6 valencys, and be leached; Oxygen is passed in reaction process, it is water-soluble that the low valence metal ion that molybdenum oxide nickel minerals can be made to produce generates high volence metal ion, high valence ion can be reused, in overall process, variable valency metal ions is equivalent to the effect of catalyzer, thus avoid the discharge of obnoxious flavour, there is the use of having saved chemical reagent.In reaction engineering, add catalyzer, contribute to the leaching yield improving molybdenum nickel, this technique is without gas reaction, and speed is controlled, environmental protection, safety.The reaction mechanism of this invention is as follows:
MoS
2+12H
2O+18Me
3+=H
2MoO
4+2SO
4 2-+22H
++18 Me
2+
MoS
2+12H
2O+18Me
3+=MoO
4 2-+2SO
4 2-+24H
++18 Me
2+
NiS
2+8Me
3++4H
2O =N
i2+2SO
4 2-+8H
++8 Me
2+
Me
2+oxidized:
Me
2++4H
++O
2=4Me
3++2H
2O
(Me is variable valency metal)
Net reaction is: 2MoS
2+ 6NiS+6H
2o+21O
2=6Ni
2+2H
2moO
4+ 10SO
4 2-+ 8H
+
The technical qualification of this invention are: under dilute sulphuric acid environment, and catalyzer is 1 ~ 2g/l in the concentration of reactor, reaction pressure 0.2 ~ 0.9MPa, PH < 5, temperature of reaction 120 ~ 160 DEG C; Reaction times 3 ~ 6h, molybdenum nickel minerals granularity 100 ~ 400 order, solid-to-liquid ratio 1:(2 ~ 6).
This technique needs to add catalyzer, certainly exists the consumption of catalyzer, adds cost, molybdenum and sulphur are leached simultaneously, in solution, there is sulfuric acid and high price molybdenum ion simultaneously, effective separation of molybdenum sulphur can not be realized, be unfavorable for effective utilization of next step molybdenum and sulphur.Therefore, develop a kind of molybdenum sulphur content that can solve the problem from method be very important.
Summary of the invention
The object of the present invention is to provide a kind of molybdenum sulphur content from method.
The object of the present invention is achieved like this, by after raw material molybdenite concentrate ball milling, insert in autoclave, add the sulphuric acid soln of solid-liquid volume ratio 4 ~ 10 times, pass at pressure 1.6 ~ 3.0MPa, temperature 160 ~ 240 DEG C oxygen reaction 8 ~ 16h realize molybdenum sulphur content from.
The present invention overcome existing molybdenite concentrate realize molybdenum sulphur isolation technique exist environment unfriendly, reagent consumption is large, production cost is high, be separated halfway deficiency, to contain molybdenum 45 ~ 55%, the molybdenite concentrate of sulfur-bearing 30 ~ 40% is raw material, dilution heat of sulfuric acid is adopted to carry out Low Pressure Oxygen leaching to molybdenite concentrate, thus realize molybdenum sulphur content from object, and provide favourable condition for next step molybdenum sulfur recovery.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
Molybdenum sulphur content of the present invention from method, by after raw material molybdenite concentrate ball milling, insert in autoclave, add the sulphuric acid soln of solid-liquid volume ratio 4 ~ 10 times, pass at pressure 1.6 ~ 3.0MPa, temperature 160 ~ 240 DEG C oxygen reaction 8 ~ 16h realize molybdenum sulphur content from.
Described ball milling is 100 ~ 300 orders by raw material molybdenite concentrate ball milling granularity.
Described raw material molybdenite concentrate is the molybdenite concentrate containing weight percent 45 ~ 55% molybdenum and 30 ~ 40% sulphur.
Described sulphuric acid soln concentration is 5 ~ 20g/L.
The described dividing potential drop passing into oxygen is 1.0 ~ 1.8MPa.
Molybdenum sulphur content of the present invention from method, be by after molybdenite concentrate ball milling, under dilute sulphuric acid environment, can in molybdenite concentrate-divalent S is first by O
2oxidation generates elemental sulfur, then by O
2oxidation generate+6 valencys, S thus generate SO
4 2-, avoid low concentration SO
2the discharge of tail gas; Pass into oxygen in reaction process, molybdenite concentrate+4 valency S can be made to be direct oxidation into the H of+6 valencys
2moO
4, H
2moO
4be insoluble to dilution heat of sulfuric acid and enter slag, thus realize molybdenum sulphur content from.This technique, without gas reaction, does not need to add catalyzer, and speed of response and time can control, and subsequent treatment process is simple, environmental friendliness.
Preferably, described concentrated molybdenum ore granularity is 100 ~ 300 orders.
Above-mentioned granularity is conducive to the leaching yield improving molybdenum and sulphur.
Preferably, described solid-to-liquid ratio is 1:(4 ~ 10).
Along with the rising of liquid-solid ratio, in molybdenite concentrate, the Oxidation Leaching rate of S and Mo also can raise, and increases the Oxidation Leaching that liquid-solid ratio is conducive to molybdenite concentrate.But cost also can significantly raise, so must by solid-to-liquid ratio in OK range.
Preferably, described dilution heat of sulfuric acid concentration is 5 ~ 20g/l.
Under different conditions, to the not obvious relation of the Oxidation Leaching rate of S, but owing to starting oxygen pressure acid leaching stage, sulfuric acid can dissolve the Mo of leaching, promotes pressure oxidation and the leaching of molybdenite concentrate, so will by Controlled acidity in OK range in beginning acid.
Preferably, the described Leaching reaction time is 8 ~ 16h.
Along with the prolongation of Leaching reaction time, the leaching yield of sulphur raises, and basic and the time is linear during beginning, after the regular hour, leaching velocity slows down, so will by the Leaching reaction time in OK range.
Preferably, it is 1.6 ~ 3.0Mpa that pressure is leached in described reaction, and oxygen partial pressure is 1.0 ~ 1.8MPa.
Along with the increase of oxygen pressure, Mo leaching yield starts to increase, and after certain degree, the change of Mo leaching yield is little, but the leaching yield of S increases with the increase of oxygen pressure substantially.But pressure increase can increase facility investment, increase production cost, so will by leaching pressure in OK range.
Preferably, described Leaching reaction temperature is 160 ~ 240 DEG C.
Along with the rising of Leaching reaction temperature, the leaching yield of Mo slightly reduces, and the leaching yield of sulphur obviously raises.Temperature increase can increase production cost, so will by Leaching reaction temperature in OK range.
Compared with prior art, tool of the present invention has the following advantages and effect:
A kind of molybdenite concentrate pressure leaching of the present invention realize molybdenum sulphur content from method, adopt acid, oxygen as oxidation system, under high-temperature and high-pressure conditions, the sulphur of Oxidation Leaching molybdenite concentrate generates sulfuric acid, and molybdenum generates molybdic acid and enters in slag, successfully achieve molybdenum sulphur content from, reaction conditions easily reaches and controls.Mechanism of the present invention is as follows:
MoS
2+3O
2+H
2O=H
2MoO
4+2S
S+1.5O
2+H
2O=H
2SO
4
Net reaction is: MoS
2+ 5/2O
2+ 3H
2o=H
2moO
4+ 2H
2sO
4
As can be seen from above reaction formula, realize in the sepn process of molybdenum sulphur at molybdenite concentrate pressure leaching, what consume only has water and oxygen, output sulfuric acid and molybdic acid.In actual production, Mo direct yield > 95%, leached mud is containing molybdenum 54 ~ 64%; The oxidation ratio > 95% of S, direct yield > 95%.A kind of molybdenite concentrate pressure leaching realize molybdenum sulphur content from method discharge without waste gas, achieve effective separation of molybdenum sulphur, for the process of next step molybdenum sulphur provides favourable condition, economic and social benefit is good.
Embodiment 1
Be 100 order molybdenite concentrate powder by 200.00g molybdenite concentrate ball milling to granularity, 98% sulfuric acid being made into concentration is 5g/l dilution heat of sulfuric acid 608mL, above-mentioned 200.00g molybdenite concentrate powder and 608mL dilution heat of sulfuric acid are joined in the autoclave of 3L, passes into oxygen and carry out Oxidation Leaching; Molybdenite concentrate main component: molybdenum grade 45%, sulphur grade 32%; Be heated to 180 DEG C, it is 1.7Mpa that pressure is leached in reaction, and oxygen partial pressure is 1.1MPa, and the reaction times is 10h.Mo direct yield 95.5%, leached mud is containing molybdenum 56%; The oxidation ratio 95.8% of S, direct yield 96.1%.
Embodiment 2
Be 300 order molybdenite concentrate powder by 200.00g molybdenite concentrate ball milling to granularity, 98% sulfuric acid being made into concentration is 20g/l dilution heat of sulfuric acid 1520mL, above-mentioned 200.00g molybdenite concentrate powder and 1520mL dilution heat of sulfuric acid are joined in the autoclave of 3L, passes into oxygen and carry out Oxidation Leaching; Molybdenite concentrate main component: molybdenum grade 55%, sulphur grade 38%; Be heated to 240 DEG C, it is 2.9Mpa that pressure is leached in reaction, and oxygen partial pressure is 1.8MPa, and the reaction times is 16h.Mo direct yield 97.7%, leached mud is containing molybdenum 63%; The oxidation ratio 98.1% of S, direct yield 97.8%.
Embodiment 3
Be 200 order molybdenite concentrate powder by 200.00g molybdenite concentrate ball milling to granularity, 98% sulfuric acid being made into concentration is 15g/l dilution heat of sulfuric acid 1216mL, above-mentioned 200.00g molybdenite concentrate powder and 1216mL dilution heat of sulfuric acid are joined in the autoclave of 3L, passes into oxygen and carry out Oxidation Leaching; Molybdenite concentrate main component: molybdenum grade 50%, sulphur grade 36%; Be heated to 220 DEG C, it is 2.3Mpa that pressure is leached in reaction, and oxygen partial pressure is 1.4MPa, and the reaction times is 12h.Mo direct yield 96.6%, leached mud is containing molybdenum 59%; The oxidation ratio 97.4% of S, direct yield 97.1%.
Embodiment 4
Be 200 order molybdenite concentrate powder by 200.00g molybdenite concentrate ball milling to granularity, 98% sulfuric acid being made into concentration is 10g/l dilution heat of sulfuric acid 912mL, above-mentioned 200.00g molybdenite concentrate powder and 912mL dilution heat of sulfuric acid are joined in the autoclave of 3L, passes into oxygen and carry out Oxidation Leaching; Molybdenite concentrate main component: molybdenum grade 51%, sulphur grade 37%; Be heated to 210 DEG C, it is 1.8Mpa that pressure is leached in reaction, and oxygen partial pressure is 1.2MPa, and the reaction times is 14h.Mo direct yield 96.2%, leached mud is containing molybdenum 58%; The oxidation ratio 97.1% of S, direct yield 96.7%.
Claims (5)
1. a molybdenum sulphur content from method, it is characterized in that after raw material molybdenite concentrate ball milling, insert in autoclave, add the sulphuric acid soln of solid-liquid volume ratio 4 ~ 10 times, pass at pressure 1.6 ~ 3.0MPa, temperature 160 ~ 240 DEG C oxygen reaction 8 ~ 16h realize molybdenum sulphur content from.
2. molybdenum sulphur content according to claim 1 from method, it is characterized in that described ball milling is is 100 ~ 300 orders by raw material molybdenite concentrate ball milling granularity.
3. molybdenum sulphur content according to claim 1 and 2 from method, it is characterized in that described raw material molybdenite concentrate is the molybdenite concentrate containing weight percent 45 ~ 55% molybdenum and 30 ~ 40% sulphur.
4. molybdenum sulphur content according to claim 1 from method, it is characterized in that described sulphuric acid soln concentration is 5 ~ 20g/L.
5. molybdenum sulphur content according to claim 1 from method, it is characterized in that the described dividing potential drop passing into oxygen is 1.0 ~ 1.8MPa.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11377365B2 (en) * | 2018-10-30 | 2022-07-05 | Molibdenos Y Metales S.A. | Process for the selective removal of copper compounds and other impurities with respect to molybdenum and rhenium, from molybdenite concentrates |
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Publication number | Priority date | Publication date | Assignee | Title |
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US11377365B2 (en) * | 2018-10-30 | 2022-07-05 | Molibdenos Y Metales S.A. | Process for the selective removal of copper compounds and other impurities with respect to molybdenum and rhenium, from molybdenite concentrates |
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Application publication date: 20150701 |