CN103305707A - Method for smelting bismuth-molybdenum or bismuth-tungsten concentrates - Google Patents

Method for smelting bismuth-molybdenum or bismuth-tungsten concentrates Download PDF

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CN103305707A
CN103305707A CN2013102560431A CN201310256043A CN103305707A CN 103305707 A CN103305707 A CN 103305707A CN 2013102560431 A CN2013102560431 A CN 2013102560431A CN 201310256043 A CN201310256043 A CN 201310256043A CN 103305707 A CN103305707 A CN 103305707A
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bismuth
molybdenum
smelting
tungsten
tungsten concentrate
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杨建广
伏彩萍
李永华
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Hunan Shizhuyuan Nonferrous Metals Co Ltd
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Hunan Shizhuyuan Nonferrous Metals Co Ltd
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Abstract

The invention provides a method for smelting bismuth-molybdenum or bismuth-tungsten concentrates. The method comprises the following steps of: firstly carrying out low-temperature sulfur fixation smelting on the bismuth-molybdenum or bismuth-tungsten concentrates, and reducing bismuth sulfide and the like in the bismuth-molybdenum or bismuth-tungsten concentrates to metal bismuth; pulping the obtained smelting slag with water; and then putting alkaline liquor obtained through liquid-solid separation of slurry into an autoclave after regulating the pH value of the alkaline liquor to undergo hydrothermal reaction to obtain molybdenum oxide or tungsten oxide. The method has the beneficial effects that problems in existing bismuth-molybdenum or bismuth-tungsten concentrate smelting processes such as heavy pollution of low-concentration SO2 and heavy metal powder, high energy consumption and low efficiency and problems in the processes for extracting molybdenum or tungsten from smelting slag such as long flow, high energy consumption, low recovery rate of molybdenum or tungsten and the like are solved; and the method has the prominent advantages of small environment stress, strong raw material adaptability, simple flow and high recovery rate of metals.

Description

A kind of smelting process for bismuth molybdenum or bismuth tungsten concentrate
Technical field
The present invention relates to field of metallurgy and chemical engineering, relate more specifically to a kind of smelting process for bismuth molybdenum or bismuth tungsten concentrate.
Background technology
China's bismuth aboundresources, reserves amount to ten thousand tons of 50-60, concentrate to be distributed in Hunan, Guangdong, Jiangxi, Yunnan Si Sheng.Wherein, the reserves of Hunan nonferrous metals ore bismuth account for national total amount 74%, have the characteristics such as of high grade, easy exploitation, are China most important bismuth raw material bases.Hunan tungsten tin molybdenum bismuth polymetallic deposit is described as mineral museum, the world, the ore resource amount of verifying reaches 3.6 hundred million tons, the mineral kind of finding reaches 143 kinds, wherein 74.6 ten thousand tons in tungsten, 31.5 ten thousand tons of bismuths, 46.8 ten thousand tons in tin, 13.0 ten thousand tons of molybdenums, 7,144 ten thousand tons of Associated Fluorite mineral deposits.Wherein, molybdenum, bismuth mainly exist with the form of molybdenum glance and bismuthinite respectively, and molybdenum glance is close with the bismuthinite flotability, and the Mo-Bi concentrate that produces has and contains mutually higher characteristics.Rely on existing flotation metallurgical technology, the difficulty that therefrom obtains qualified molybdenum, bismuth converted products is increasing, only can be contained mutually higher concentrated molybdenum ore or bismuth concentrate product.Therefore, in the urgent need to developing new separation and recovery technology.
Bismuth molybdenum (or tungsten) the concentrate separation and recovery technology of new development is except must realizing also must satisfying the requirements such as technical process is short, energy consumption is low, environmental stress is little the high efficiency separation of bismuth, molybdenum (or tungsten).But bismuth molybdenum (or tungsten) the concentrate method of open report or stress the simple separation of bismuth, molybdenum and ignored the depth extraction of bismuth molybdenum so far, or have that technical process is long, energy consumption is high, environmental pollution heavily waits shortcoming.
For example, Chinese patent CN201210128588.X discloses and a kind ofly electrooxidation is carried out in molybdenum glance and bismuthinite mixing ore deposit has leached the method separate.Namely, bismuthinite concentrate or the chats product that will contain molybdenum carry out diaphragm-free electrolysis in the chloride soln of pH＞7, molybdenum ore is entered liquid phase by the selectivity oxygenolysis, obtain the molybdate aqueous solution, bismuthinite then can not oxidation and is stayed in the solid phase, after the filtering separation, obtain comparatively single bismuthinite mineral.The method can realize separating of molybdenum glance and bismuthinite preferably, but the bismuthinite of gained also must further be processed just and can obtain the bismuth metal product; Chinese patent CN201110296797.0 has mentioned a kind of wet separation technique of leaded bismuth molybdenum material, be about to leaded bismuth molybdenum material first through ball milling, add soda ash and oxygenant slurrying, the leaching of heating of slurrying feed liquid, molybdenum is present in the leach liquor with the Sodium orthomolybdate form, and lead, bismuth, silver, copper and iron are stayed and are formed plumbous bismuth silver copper scum in the leached mud; Leach liquor is partly dissolved lead with hydrochloric acid acidizing and precipitation, forms lead skim and reclaims with plumbous pyrometallurgical smelting, adds calcium chloride again, is settled out calcium molybdate; Above-mentioned leaded bismuth silver copper scum leaches with sulfuric acid, sodium-chlor, hydrogen peroxide, and Pb is with the isolated in form of argentalium slag; Heavy plumbous rear liquid is by the heavy bismuth of hydrolysis; Thereby realize the separation of lead, bismuth, molybdenum.The problems such as there is long flow path in the method, and environmental stress is large.
Summary of the invention
The purpose of this invention is to provide a kind of smelting process that is used for bismuth molybdenum or bismuth tungsten concentrate that can reduce cost and energy-saving and emission-reduction.
To achieve these goals, the invention provides a kind of technical scheme: a kind of smelting process for bismuth molybdenum or bismuth tungsten concentrate, it may further comprise the steps:
1) bismuth molybdenum or bismuth tungsten concentrate are carried out the melting of low-temperature solid sulphur
The condition of melting is: smelting temperature is 750-950 ℃, selects metal oxide as sulphur-fixing agent, and the add-on of metal oxide with the 1-5 of required theoretical amount when the contained S of bismuth sulfide all is converted into metallic sulfide in bismuth molybdenum or the bismuth tungsten concentrate is doubly selected Na 2CO 3As reaction flux, its add-on is bismuth molybdenum or bismuth tungsten concentrate quality 1-8 times, selects fine coal or coke as reductive agent, and its consumption is the 5-20% of bismuth molybdenum or bismuth tungsten concentrate quality, and smelting time is 30 min-180 min;
2) bismuth molybdenum or bismuth tungsten concentrate low-temperature solid sulphur smelting slag are carried out the pulp processing
The condition of pulp is: take tap water as slurry reagent, the pulp temperature is 20-90 ℃, and the time is 10 min-120 min, and the liquor capacity take ml as unit and the metallurgical slag mass ratio take g as unit are 1-5:1;
3) slurry after the pulp is carried out hydrothermal deposition
At first slurry is carried out liquid-solid separation, obtain metallic sulfide concentrate and alkali lye, be 7-9 with alkali lye pH adjusted value again, place autoclave to carry out hydrothermal deposition the solution behind the adjustment pH, the condition of hydrothermal deposition is: 260 ℃-500 ℃ of temperature, pressure 5MPa-40MPa, times 10 min-600 min separates out MoO3 or WO3 powder at last.
Described metal oxide is ZnO or CuO.
Described 1) gets 100g bismuth concentrated molybdenum ore and 70g ZnO, 300g Na in 2CO 3Reaching 8g fine coal and mix, is 870 ℃ of lower melting 120min at smelting temperature.
Described 2) add the 600ml tap water in cooled smelting slag, pulp temperature 60 C, slurry time 60min.
Described 3) the liquid-solid separation of slurry in, obtain containing pulp slag and the alkali lye of 71.3% ZnS, alkali lye is adjusted to be placed on about pH to 8 with concentrated hydrochloric acid and is carried out hydrothermal deposition in the autoclave, 330 ℃ of hydrothermal temperatures, pressure 20MPa, time 180min is after reaction finishes, the solution cold filtration separates, and obtains 6.12g molybdenum oxide hydrate powder MoO 3XH 2O.
Compared with prior art, technical scheme of the present invention has following beneficial effect:
(1) bismuth molybdenum or bismuth tungsten concentrate so that the bismuth in bismuth molybdenum or the bismuth tungsten concentrate restores being significantly less than under the condition of existing smelting temperature, have reduced energy consumption at first by low-temperature solid sulphur melting reaction among the present invention.
(2) metal in the described metal oxide that is added into of the S in bismuth molybdenum or the bismuth tungsten concentrate is fixed, and forms more stable metallic sulfide, has avoided existing smelting process low concentration SO 2The problem of refractory reason.
(3) alkaline residue that obtains after the low-temperature solid reaction of Salmon-Saxl finishes obtains alkali lye after pulp, liquid-solid separation directly carries out hydrothermal deposition and obtains MoO 3Or WO 3Powder has then been avoided existing bismuth molybdenum or bismuth tungsten concentrate " soda ash leaching-sulfide precipitation-sulfidation roasting " technique to have long flow path, has been polluted the shortcoming heavy, that the rate of recovery is low; The present invention has realized low-carbon (LC), cleaning and the high efficiente callback of bismuth molybdenum or bismuth tungsten concentrate by the combination of " melting of low-temperature solid sulphur "+" hydrothermal deposition ".
Description of drawings
Fig. 1 is the process flow sheet that the present invention is used for the smelting process of bismuth molybdenum or bismuth tungsten concentrate.
Embodiment
Following content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that implementation of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
As shown in Figure 1, be process flow sheet of the present invention, MeO represents a kind of metal oxide, and MeS represents a kind of metallic sulfide, and concrete steps and principle are:
1. the low-temperature solid sulphur melting of bismuth molybdenum or bismuth tungsten concentrate
Bismuth sulfide in bismuth molybdenum or the bismuth tungsten concentrate is reduced to bismuth with elementary:
2Bi2S3+6MeO+3C＝4Bi+6MeS+3CO 2
In bismuth molybdenum or the bismuth tungsten concentrate tungsten, molybdenum component then be converted into Na 2MoO 4Or Na 2WO 4Deng:
2MoS 2+2Na 2CO 3+4MeO+O 2=2Na 2MoO 4+4MeS+2CO 2
CaWO 4+Na 2CO 3=CaCO 3+Na 2WO 4
H 2WO 4+Na 2CO 3=Na 2WO 4+H 2O+CO 2
Following reaction occurs in the impurity composition in bismuth molybdenum or the bismuth tungsten concentrate:
2Ag 2S+2MeO+C=4Ag+2MeS+CO 2
2PbS+2MeO+C=2Pb+2MeS+CO 2
2Cu 2S+2MeO+C=4Cu+2MeS+CO 2
2FeS 2+4MeO+C=2FeO+4MeS+CO 2
Me in the system 2S 3Also may with Na 2CO 3Following reaction occurs:
2Me 2S 3+6Na 2CO 3+3C=4Me+6Na 2S+9CO 2
But the Na that reaction generates 2S thereupon with system in MeO following reaction occurs, realized Na 2CO 3Regeneration, also be the Na in the system 2CO 3Keep the reaction front and back constant, only provide a kind of inert reaction medium for the melting of low-temperature solid sulphur:
Na 2S+MeO+CO 2=Na 2CO 3+MeS
2. the pulp of metallurgical slag
The pulp process can realize Na 2MoO 4Or Na 2WO 4From metallurgical slag, separate.Sulfur retention products MeS stays in the slag with the gangue content etc. that has neither part nor lot in reaction, and the Na that reaction generates 2MoO 4Or Na 2WO 4Then with Na 2CO 3Enter alkali lye.
3. hydrothermal deposition
Alkali lye is after adjusting the pH value, and following reaction occurs under hydrothermal condition for molybdate or wolframate radical, generates molybdenum oxide or tungstic oxide hydrate, obtains molybdenum oxide or oxidation tungsten powder through further dewatering.
H ++ MoO 4 2- Hydro-thermal → MoO 3XH 2O
H ++ WO 4 2- Hydro-thermal → WO 3XH 2O
Embodiment one:
The molybdenum bismuth concentrate composition that provides is: Bi 21.02%, and Mo 5.33%, and Fe 13.24%, SiO 214.56%, Cu 0.77%, and S 27.2%.
Get above-mentioned molybdenum bismuth fine ore 100g, with 70g ZnO, 300g Na 2CO 3And 8g fine coal batch mixing is even, melting 120 min under 870 ℃ of conditions.After reaction finished, refrigerated separation obtained thick bismuth 18.5g, through chemical analysis bismuth grade 97.24%.Add the 600ml tap water in cooled smelting slag, shear agitation pulp, pulp temperature 60 C, slurry time 60min.Afterwards, the liquid-solid separation of slip obtains respectively containing pulp slag and the alkali lye of 71.3% ZnS.Alkali lye is adjusted to be placed on about pH to 8 with concentrated hydrochloric acid and is carried out hydrothermal deposition in the autoclave, 330 ℃ of hydrothermal temperatures, pressure 20MPa, time 180min.After reaction finished, the solution cold filtration separated, and obtains 6.12g molybdenum oxide hydrate powder MoO 3XH 2O.
Embodiment two:
The bismuth tungsten concentrate composition that provides is: Bi 16.45%, WO 33.17%, Fe 20.19%, SiO 26.21%, Cu 0.14%, and S 21.5%.
Get above-mentioned tungsten bismuth fine ore 100g, with 90g ZnO, 500g Na 2CO 3And 12g fine coal batch mixing is even, melting 90 min under 950 ℃ of conditions.After reaction finished, refrigerated separation obtained thick bismuth 15.27g, thick bismuth grade 96.11%.Add the 1000ml tap water in cooled smelting slag, shear agitation pulp, 75 ℃ of pulp temperature, slurry time 90min.Afterwards, slurry filtration obtains containing pulp slag and the alkali lye of 73.17% ZnS, and alkali lye is adjusted pH as about 9 take acetic acid.Place autoclave to carry out hydrothermal deposition the solution that mixes up behind the pH, 360 ℃ of hydrothermal temperatures, pressure 22MPa, times 240 min.After reaction finished, the solution cold filtration separated, and obtains tungstic oxide hydrate powder (WO 3XH 2O) 3.97g.
Embodiment three:
The chemical constitution of the bismuth concentrated molybdenum ore that provides is (%): Bi 25.29, Mo 3.11, Fe 19.4, S 26.1, Cu 0.2, Pb 0.49, SiO 26.13.
Taking by weighing respectively 1000g molybdenum bismuth concentrate, 100g coke, the cupric oxide cigarette ash 850g that contains Cu 71% and 4000g yellow soda ash evenly mixes.At 750 ℃ of lower melting 2 h, output contains the thick bismuth 249g of Bi 98.2%; Add the pulp under the condition of 90 ℃ of temperature, time 2h of 4000mL tap water after the cooling, afterwards, slurry filtration obtains respectively containing pulp slag and the alkali lye of 61.4% CuS.Alkali lye is adjusted pH as about 9 take 50% concentrated nitric acid.Place autoclave to carry out hydrothermal deposition the solution that mixes up behind the pH, 350 ℃ of hydrothermal temperatures, pressure 21MPa, time 400min.After reaction finished, the solution cold filtration separated, and obtains molybdenum oxide hydrate powder (MoO 3XH 2O) 42.8g.
Bismuth molybdenum or bismuth tungsten concentrate be at first by low-temperature solid sulphur melting reaction among the present invention, so that the bismuth in bismuth molybdenum or the bismuth tungsten concentrate restores being significantly less than under the condition of existing smelting temperature, reduced energy consumption; Simultaneously, the ZnO that the S in bismuth molybdenum or the bismuth tungsten concentrate is added into or the metal among CuO or the MeO are fixed, and form more stable ZnS or CuS or MeS, have avoided existing smelting process low concentration SO 2The problem of refractory reason; In addition, as the Na that reacts flux 2CO 3Character is constant before and after reaction, only provides a kind of inert reaction medium for the low-temperature solid reaction of Salmon-Saxl.And the alkaline residue that the low-temperature solid reaction of Salmon-Saxl obtains after finishing obtains alkali lye and directly carries out hydrothermal deposition and obtain MoO after pulp, liquid-solid separation 3Or WO 3Powder has then been avoided existing bismuth molybdenum or bismuth tungsten concentrate " soda ash leaching-sulfide precipitation-sulfidation roasting " technique to have long flow path, has been polluted the shortcoming heavy, that the rate of recovery is low.The present invention has realized low-carbon (LC), cleaning and the high efficiente callback of molybdenum (or tungsten) bismuth concentrate by the combination of " melting of low-temperature solid sulphur "+" hydrothermal deposition ".
In a word, the present invention compares with existing bismuth molybdenum or bismuth tungsten concentrate smelting technology, not only greatly reduce cost, reduced energy consumption, realize the effective separation of bismuth molybdenum or bismuth tungsten and other valuable metal element, and reduced the discharging of " three wastes ", accomplished cleaner production, effects of energy saving and emission reduction is obvious, has significant economic benefit and social benefit.

Claims (5)

1. smelting process that is used for bismuth molybdenum or bismuth tungsten concentrate is characterized in that: may further comprise the steps:
1) bismuth molybdenum or bismuth tungsten concentrate are carried out the melting of low-temperature solid sulphur
The condition of melting is: smelting temperature is 750-950 ℃, selects metal oxide as sulphur-fixing agent, and the add-on of metal oxide with the 1-5 of required theoretical amount when the contained S of bismuth sulfide all is converted into metallic sulfide in bismuth molybdenum or the bismuth tungsten concentrate is doubly selected Na 2CO 3As reaction flux, its add-on is bismuth molybdenum or bismuth tungsten concentrate quality 1-8 times, selects fine coal or coke as reductive agent, and its consumption is the 5-20% of bismuth molybdenum or bismuth tungsten concentrate quality, and smelting time is 30 min-180 min;
2) bismuth molybdenum or bismuth tungsten concentrate low-temperature solid sulphur smelting slag are carried out the pulp processing
The condition of pulp is: take tap water as slurry reagent, the pulp temperature is 20-90 ℃, and the time is 10 min-120 min, and the liquor capacity take ml as unit and the metallurgical slag mass ratio take g as unit are 1-5:1;
3) slurry after the pulp is carried out hydrothermal deposition
At first slurry is carried out liquid-solid separation, obtain metallic sulfide concentrate and alkali lye, be 7-9 with alkali lye pH adjusted value again, place autoclave to carry out hydrothermal deposition the solution behind the adjustment pH, the condition of hydrothermal deposition is: 260 ℃-500 ℃ of temperature, pressure 5MPa-40MPa, times 10 min-600 min separates out MoO3 or WO3 powder at last.
2. the smelting process for bismuth molybdenum or bismuth tungsten concentrate as claimed in claim 1, it is characterized in that: described metal oxide is ZnO or CuO.
3. the smelting process for bismuth molybdenum or bismuth tungsten concentrate as claimed in claim 2 is characterized in that: get 100g bismuth concentrated molybdenum ore and 70g ZnO, 300g Na described 1) 2CO 3Reaching 8g fine coal and mix, is 870 ℃ of lower melting 120min at smelting temperature.
4. the smelting process for bismuth molybdenum or bismuth tungsten concentrate as claimed in claim 3 is characterized in that: add the 600ml tap water described 2) in cooled smelting slag, pulp temperature 60 C, slurry time 60min.
5. the smelting process for bismuth molybdenum or bismuth tungsten concentrate as claimed in claim 4, it is characterized in that: the liquid-solid separation of slurry described 3), obtain containing pulp slag and the alkali lye of 71.3% ZnS, alkali lye is adjusted to be placed on about pH to 8 with concentrated hydrochloric acid and is carried out hydrothermal deposition in the autoclave, 330 ℃ of hydrothermal temperatures, pressure 20MPa, time 180min, after reaction finished, the solution cold filtration separated, and obtains 6.12g molybdenum oxide hydrate powder MoO 3XH 2O.
CN2013102560431A 2013-06-25 2013-06-25 Method for smelting bismuth-molybdenum or bismuth-tungsten concentrates Pending CN103305707A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105803224A (en) * 2016-03-10 2016-07-27 中南大学 One-step clean bismuth smelting method for complex bismuth sulfide ore
CN109881016A (en) * 2019-04-24 2019-06-14 江西理工大学 The method that a kind of disposition of soda boiling tungsten slag harmlessness and valuable metal extract
CN110016563A (en) * 2019-04-24 2019-07-16 江西理工大学 A kind of method of pyrocarbon vat black tungsten slag higher value application

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Publication number Priority date Publication date Assignee Title
CN101289710A (en) * 2008-06-16 2008-10-22 中南大学 Process for abstracting bismuth by low-temperature alkaline fusion metallurgy of bismuth clean ore
CN101956084A (en) * 2010-06-28 2011-01-26 中南大学 Low temperature molten salt clean metallurgy method of bismuth

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101289710A (en) * 2008-06-16 2008-10-22 中南大学 Process for abstracting bismuth by low-temperature alkaline fusion metallurgy of bismuth clean ore
CN101956084A (en) * 2010-06-28 2011-01-26 中南大学 Low temperature molten salt clean metallurgy method of bismuth

Non-Patent Citations (1)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105803224A (en) * 2016-03-10 2016-07-27 中南大学 One-step clean bismuth smelting method for complex bismuth sulfide ore
CN109881016A (en) * 2019-04-24 2019-06-14 江西理工大学 The method that a kind of disposition of soda boiling tungsten slag harmlessness and valuable metal extract
CN110016563A (en) * 2019-04-24 2019-07-16 江西理工大学 A kind of method of pyrocarbon vat black tungsten slag higher value application
CN110016563B (en) * 2019-04-24 2020-11-06 江西理工大学 High-value utilization method of high-temperature carbon reduction black tungsten slag
CN109881016B (en) * 2019-04-24 2021-07-09 江西理工大学 Method for harmless treatment of alkali-boiled tungsten residues and extraction of valuable metals

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