CN204417566U - A kind of device processing antimony arsenic material - Google Patents

A kind of device processing antimony arsenic material Download PDF

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Publication number
CN204417566U
CN204417566U CN201520044509.6U CN201520044509U CN204417566U CN 204417566 U CN204417566 U CN 204417566U CN 201520044509 U CN201520044509 U CN 201520044509U CN 204417566 U CN204417566 U CN 204417566U
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arsenic
antimony
refractory masses
plumbago crucible
volatile matter
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CN201520044509.6U
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陈正
惠应武
郭键柄
张琪
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Lanzhou Engineering and Research Institute of Nonferrous Metallurgy Co Ltd
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Lanzhou Engineering and Research Institute of Nonferrous Metallurgy Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The utility model discloses a kind of device processing antimony arsenic material, to solve the problem that detrimental impurity arsenic in antimony arsenic material smelting process is difficult to remove.This device comprises body of heater, bell, shaft, tubular refractory masses is provided with in body of heater, the center of described refractory masses is placed with plumbago crucible, refractory masses top is placed with volatile matter receiving tank, volatile matter receiving tank is positioned at the top outer of plumbago crucible, leave gap between volatile matter receiving tank and plumbago crucible, the bottom of refractory masses is connected with vacuum pump by vacuum pump line, is provided with heating system between plumbago crucible and refractory masses.The utility model, based on vacuum metallurgy principle, achieves antimony in antimony arsenic alloy material and is separated with the effective of arsenic, treating processes clean and effective, produces without waste water and dregs, and avoid the secondary pollution of arsenic, simultaneously metal recovery rate is high.

Description

A kind of device processing antimony arsenic material
Technical field
The utility model belongs to non-ferrous metallurgy technology field, is specifically related to a kind for the treatment of unit of antimony arsenic material.
Background technology
Shi Chan antimony big country of China is also the country that antimony resource is the abundantest in the world, and antimony reserves account for 32.9% of world's antimony reserves.But through the exploitation of decades, single the available of antimony type ore finds out that resource reserve reduces year by year, Backup Base is not enough, and mixed type antimony ore thus must be turned to as the development and utilization of plumbous antimony ore, antimony arsenic minerals etc.The exploitation of mixed type antimony ore and utilization create a large amount of antimony arsenic alloies.Arsenic is a kind of extremely harmful impurity element, and volatilization reacts with the oxygen in air and generates white arsenic (As at ambient pressure 2o 3) i.e. arsenic, toxicity is very large, can cause damage to operator's health.Not only affect the economic and technical norms in smelting system, more cause severe contamination to environment.Because antimony arsenic is arranged in the same main group of the periodic table of elements, the metallic state of antimony and arsenic can infinitely dissolve each other, and brings difficulty to the arsenic removal of antimony arsenic alloy.
The main method of current needle antimony arsenic removal has basic refining arsenic removal method, adds aluminium arsenic removal method, aqueous electrolysis refining arsenic removal method etc.
Oxidation basic refining arsenic removal method is the main method of current needle antimony arsenic removal.At 1073 ~ 1123K temperature, add Na by arsenic cubage 2cO 3or add NaOH:Na 2cO 3the mixed flux of=1:3, in antimony liquid, blast air, arsenic is oxidized to As 2o 5, then with slag former Na 2cO 3reaction, generates sodium arseniate (Na 3asO 4) and a small amount of Sodium metaarsenite (Na 3asO 3) and be separated with antimony.
The arsenic alkali slag that the method produces is poisonous, and it is stacked and process all has problems.Meanwhile, in refining process, antimony also generates sodium antimonate and enters arsenic alkali slag, and general every kg arsenic will take away 5-10 kg antimony, and the consumption of antimony is large, is separated comparatively complicated further.
Adding aluminium arsenic removal method is under certain operating mode, mainly utilizes arsenic aluminium can form the principle arsenic removal of arsenic aluminium alloy in the molten state, how to apply when tin refinement, following [As]+[the Al]=AlAs (s) of reaction.(AlAs) scum silica frost that the method produces is poisonous, and Al is expensive, and production cost is high.
The electrolysis arsenic removal that aqueous electrolysis method is more traditional improves current density, reduces electrolysis temperature, and add disodium ethylene diamine tetraacetate to suppress the dissolving of arsenic at anode and the precipitation at negative electrode, can obtain qualified negative electrode antimony, last arsenic enters in the anode sludge simultaneously.This method is still in the laboratory study stage, and throughput is little, and power consumption is high, and ionogen adds hydrofluoric acid, requires higher to electrolyzer material, also needs to solve the problems such as circulation of elecrolyte simultaneously.
Utility model content
The purpose of this utility model is to provide a kind of device processing antimony arsenic material, to solve the problem that detrimental impurity arsenic in antimony arsenic material smelting process is difficult to remove.
The technical solution adopted in the utility model is as follows: a kind of device processing antimony arsenic material, comprise body of heater, bell, shaft, tubular refractory masses is provided with in body of heater, the center of described refractory masses is placed with plumbago crucible, refractory masses top is placed with volatile matter receiving tank, volatile matter receiving tank is positioned at the top outer of plumbago crucible, gap is left between volatile matter receiving tank and plumbago crucible, the bottom of refractory masses is connected with vacuum pump by vacuum pump line, heating system is provided with between plumbago crucible and refractory masses, sealing-ring is provided with between bell and shaft.
Preferably, described bell and shaft, with chuck, are provided with water composite cooling pipe in chuck, water composite cooling pipe water receiving cooling system.
Preferably, the bottom of described plumbago crucible is provided with temperature thermocouple.
Preferably, described heating system is resistive heater.
Ultimate principle of the present utility model: utilizing the utility model device process antimony arsenic material, is in fact vacuum distilling sepn process.Because the boiling point of arsenic is close to 615 DEG C, the boiling point of antimony 1635 DEG C, the saturated vapor pressure difference of antimony and arsenic is large.Fig. 1 is Sb-As system binary phase diagram, and as seen from the figure, Sb-As ties up in full compositing range and do not generate compound, completely mutually dissolves, also mutually dissolve time solid-state time liquid, is forming azeotropic mixture containing As19.5% place.Under a certain pressure, azeotropic mixture has definite composition, can not carry out Separation of Mixtures with Same Boiling Point with fractionating method; But when external pressure changes, the composition of azeotropic mixture also becomes, fractionation also can reach separating-purifying on rare occasion, and particularly at rich antimony end, the needle antimony containing As < 19.5% can not affect the volatilization removing of arsenic.Therefore, utilize the difference of antimony and arsenic saturated vapor pressure, control that suitable distillation temperature is low, distillation time and pressure (vacuum tightness), the fractionation by distillation of antimony arsenic material can be realized.After distillation, arsenic vapour condensation is with the form output of metallic arsenic, and toxicity is minimum, and economic worth is high, avoids the secondary pollution that in traditional needle antimony arsenic removal process, arsenic salt brings.
The utility model is based on vacuum metallurgy principle, adopt a kind of vacuum distillation plant process antimony arsenic material, achieve arsenic in antimony arsenic material and be separated with the effective of antimony, treating processes clean and effective, to produce without waste water and dregs, avoid the secondary pollution of arsenic, metal recovery rate is high simultaneously; The metallic antimony obtained and metallic arsenic product, the toxicity of metallic arsenic is low, the secondary pollution that when effectively can solve coarse antimony refining, arsenic impurities brings, and what realize antimony arsenic material cleans process, reduces enterprise's production cost, improves enterprise profit.
The whole treating processes of the utility model produces without slag and effluent, and during discharging, arsenic is metallic arsenic, and its toxicity of oxide compound comparing arsenic is minimum.Whole antimony arsenic separation process scheme is short, and do not need to add other chemical reagent and just can obtain metallic arsenic and metallic antimony two kinds of price products, compare with electrorefining with pyrorefining, the utility model advantageously.
The utility model can realize the removal of harmful element arsenic in antimony arsenic alloy, and in needle antimony, arsenic can drop to less than 1% through single flash, and antimony recovery is higher, and separating effect is obvious.Adopt the process of the utility model device to contain the more antimony arsenic alloy material of arsenic, produce without harmful waste water waste residue, treating processes energy-saving and environmental protection.
The utility model has the advantage of:
(1) treating processes clean environment firendly, non-secondary pollution.The utility model completes under vacuum conditions, and treating processes seals completely.Harmful element arsenic first with the volatilization of the form of arsenic steam, is finally condensed into metallic arsenic and concentrates on volatile matter receiving tank in vacuum oven, compares traditional arsenic removal method and produces without harmful waste water waste residue, non-secondary pollution.
(2) the utility model vacuum tightness is 300Pa-500Pa, belongs to low vacuum.
(3) technical process is short: the utility model only needs single flash can realize the removal of detrimental impurity arsenic in antimony arsenic material, and technical process is brief.
(4) product economy is worth high.After traditional antimony arsenic is separated, arsenic is with the form output of arsenic salt, and arsenic salt poisonous and harmful, economic worth is low.The product of the utility model arsenic is metallic arsenic, and toxicity is little, and economic worth is high.
(5) metal recovery rate is high.The utility model carries out in vacuum oven, and vacuum environment lower furnace body seals completely, and treating processes metal quality balances, not loss, and metal recovery rate is high.
(6) energy consumption is low.The utility model process antimony arsenic material, low vacuum; Treatment unit only adopts electrically heated.Therefore, Traditional Method energy consumption is compared low.
Accompanying drawing explanation
Fig. 1 is Sb-As system binary phase diagram;
Fig. 2 is a kind of structural representation processing the device of antimony arsenic material.
Reference numeral implication is as follows: body of heater (1), bell (2), shaft (3), volatile matter receiving tank (4), refractory masses (5), plumbago crucible (6), resistive heater (7), temperature thermocouple (8), vacuum pump line (10), sealing-ring (11), water composite cooling pipe (12).
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in more detail.
A kind of device processing antimony arsenic material, comprise body of heater 1, bell 2, shaft 3, tubular refractory masses 5 is provided with in body of heater 1, the center of refractory masses 5 is placed with plumbago crucible 6, and refractory masses 5 top is placed with volatile matter receiving tank 4, and volatile matter receiving tank 4 is positioned at the top outer of plumbago crucible 6, gap is left between volatile matter receiving tank 4 and plumbago crucible 6, the bottom of refractory masses 5 is connected with vacuum pump by vacuum pump line 10, and vacuum pump is existing apparatus, and accompanying drawing does not mark; Be provided with heating system between plumbago crucible 6 and refractory masses 5, in present embodiment, heating system adopts resistive heater 7, but is not limited to this kind of type of heating, also comprises induction heating mode etc.Sealing-ring 11 is provided with between bell 2 and shaft 3.External application bolt links, and is convenient to dismounting, reinforced and feeding.The bottom of plumbago crucible 6 is provided with temperature thermocouple 8.
Bell 2 and shaft 3, with chuck (adopting double-layer stainless steel material), are provided with water composite cooling pipe 12, water composite cooling pipe 12 water receiving cooling system (existing apparatus, accompanying drawing does not mark) in chuck.
For safety, first vacuumize and reheat, heating front opening water cooling system, prevents graphite material in stove from burning out when hot environment.Vacuumize while heat up.
Arsenic is finally condensate in volatile matter receiving tank with the form preferential volatilization of metallic arsenic, and antimony is then condensate in plumbago crucible with the form of metallic antimony, does not have waste water and dregs output, non-secondary pollution.
Example. raw materials used is a kind of antimony arsenic alloy, and its main chemical compositions is antimony and arsenic, has a small amount of lead, composition in table 1, main technical details: distillation temperature 950 DEG C, soaking time 30min, vacuum tightness 500Pa.
Specific works process is as follows:
(1) reinforced: pending antimony arsenic material to be added plumbago crucible in stove (6), covers bell (2), sealing body of heater;
(2) vacuumize: by body of heater fit sealing, open vacuum pump evacuation, when in stove, vacuum tightness reaches 300Pa-500Pa, heating system heats, and limit heating edge vacuumizes;
(3) heat up: cooling system of fetching boiling water, heat up to body of heater while vacuum pump runs, make in-furnace temperature between 800 DEG C-950 DEG C, continue to vacuumize;
(4) be incubated: keep temperature 800 DEG C-950 DEG C, adjustment heating power, insulation 30-90 min, continue to vacuumize;
(5) lower the temperature: after described step (4) completes, close heating power supply, until in-furnace temperature is down to room temperature;
(6) discharging: close vacuum pump and open its purging valve, closes water-cooling system, opens bell, takes out the volatile matter in volatile matter receiving tank and the steaming debris getting in plumbago crucible respectively.
Because in alloy, arsenic impurities amount is few and volatile, only weigh steaming debris getting, chemically examine, from result, after single flash, in antimony alloy, arsenic content has been reduced to 0.49-0.93% by 6.44%, and antimony recovery 96.45-99.72%, separating effect is better.

Claims (4)

1. one kind processes the device of antimony arsenic material, it is characterized in that: it comprises body of heater (1), bell (2), shaft (3), tubular refractory masses (5) is provided with in body of heater (1), the center of described refractory masses (5) is placed with plumbago crucible (6), refractory masses (5) top is placed with volatile matter receiving tank (4), volatile matter receiving tank (4) is positioned at the top outer of plumbago crucible (6), gap is left between volatile matter receiving tank (4) and plumbago crucible (6), the bottom of refractory masses (5) is connected with vacuum pump by vacuum pump line (10), heating system is provided with between plumbago crucible (6) and refractory masses (5), sealing-ring (11) is provided with between bell (2) and shaft (3).
2. a kind of device processing antimony arsenic material according to claim 1, is characterized in that: described bell (2) and shaft (3), with chuck, are provided with water composite cooling pipe (12) in chuck, water composite cooling pipe (12) water receiving cooling system.
3. a kind of device processing antimony arsenic material according to claim 1 and 2, is characterized in that: the bottom of described plumbago crucible (6) is provided with temperature thermocouple (8).
4. a kind of device processing antimony arsenic material according to claim 3, is characterized in that: described heating system is resistive heater (7).
CN201520044509.6U 2015-01-22 2015-01-22 A kind of device processing antimony arsenic material Active CN204417566U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561605A (en) * 2015-01-22 2015-04-29 兰州有色冶金设计研究院有限公司 Device and method for treating antimony-arsenic materials
CN111979419A (en) * 2020-09-15 2020-11-24 中山智隆新材料科技有限公司 Purification device for purifying indium from ITO waste target

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561605A (en) * 2015-01-22 2015-04-29 兰州有色冶金设计研究院有限公司 Device and method for treating antimony-arsenic materials
CN104561605B (en) * 2015-01-22 2016-06-15 兰州有色冶金设计研究院有限公司 A kind of device processing antimony arsenic material
CN111979419A (en) * 2020-09-15 2020-11-24 中山智隆新材料科技有限公司 Purification device for purifying indium from ITO waste target

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