CN104109766A - Technology for separating and purifying bismuth from lead-bismuth alloy - Google Patents
Technology for separating and purifying bismuth from lead-bismuth alloy Download PDFInfo
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- CN104109766A CN104109766A CN201410373065.0A CN201410373065A CN104109766A CN 104109766 A CN104109766 A CN 104109766A CN 201410373065 A CN201410373065 A CN 201410373065A CN 104109766 A CN104109766 A CN 104109766A
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Abstract
The invention discloses a technology for separating and purifying bismuth from lead-bismuth alloy. The technology comprises the following steps: continuously carrying out vacuum distillation by adopting a vacuum distillation furnace system to separate and purify bismuth, wherein the vacuum distillation furnace consists of a melting furnace, a siphon tank and a vacuum distillation furnace; firstly continuously conveying the lead-bismuth alloy into a melting furnace body, melting, then conveying into the vacuum distillation furnace, carrying out vacuum distillation so as to separate and purify the bismuth. The purity of bismuth obtained by separation can achieve more than 99.9%, the produced lead alloy has no bismuth residues, and the continuous separation of bismuth in the lead-bismuth alloy can be realized; the technology is low in cost, low in energy consumption and environment-friendly, thus meeting the industrial production requirements.
Description
Technical field
The present invention relates to a kind of from lead bismuth alloy the technique of separating-purifying bismuth, belong to bismuth and smelt purification technique field.
Background technology
Bismuth (bismuth), ordination number 83, silvery white or blush, have metalluster.Mainly for the manufacture of fusible alloy, for scolding tin, safety fuse, fire protection system, automatic water sprayer, boiler safety plug etc.Meanwhile, bismuth alloy has non-shrinking characteristic of while solidifying, for casting printing font and high precision casting mold.In addition, bismuthyl carbonate and bismuthyl nitrate are used for the treatment of skin injury and gastroenteropathy.
Lead bismuth alloy, in nonferrous smelting or iron work, many times with byproduct, occur, its economic worth, use value are all little, need be isolated, purify, become lead bullion, smart bismuth, its use value of competence exertion and economic worth, through scientific worker and technical specialist's long-felt, current domestic lead, bismuth isolation technique mainly be take chlorination process and electrolytic process as main.Chlorination process Gai Fa Large scale nonferrous metals smeltery is used more.Its production process is by lead bismuth alloy fusing, in melt, leads to people's chlorine, and plumbous preferential and chlorine chemical combination formation chlorination lead skim (plumbous Cl2), removes chlorination lead skim, thereby reach separation of lead bismuth.The bismuth separating, again through pyrogenic attack, obtains smart bismuth.Meanwhile, chlorination lead skim otherwise processed, output lead bullion.Advantage: (1) this method is fairly simple, is applicable to scale operation.Shortcoming: (1) this method method cost is higher, needs shape large-scale production just to produce economic worth.(2), in alloy during content≤12% of bismuth, this method cost can be very high, industrial production application.(3) operational requirement is strict, easy contaminate environment, and environment toxic is large.(4) after chlorination, bismuth and lead all need again to smelt, and cause total cost to rise, and continue to cause environmental pollution.Electrolytic process, after being about to alloy and dissolving, after the certain mother liquor of adapted, according to plumbous, bismuth standard potential difference take electrolytic process.Under certain conditions such as electrolysis voltage, the lead in alloy anode plate forms ion and dissolves in electrolytic solution, and on lead electrode plate, reduces and separate out electric plumbous product subsequently, general lead >=99.5%; And bismuth has more positive polarity than lead, not there is not electrochemical solution and form anode sludge enrichment, general bismuth >=95%, i.e. thick bismuth.Thick bismuth just can obtain smart bismuth with pyrorefining again.Advantage: (1) cost is relatively low.(2) equipment investment is relatively less.Shortcoming: (1) mother liquor is selected more crucial, otherwise easily causes electric plumbous foreign matter content to increase, thereby the low grade of electrolytic efficiency causes sepn process not reach requirement.(2) owing to being electrolysis, its energy consumption is relatively high.(3) bismuth also needs further processing after forming the anode sludge, causes follow-up environmental pollution.(4), due to the water contaminative of electrolysis waste solution, after need dealing with, could discharge.(5) electrolytic process is applicable to the alloy that bismuth-containing amount is lower.
Summary of the invention
The defect existing in technology for chlorination process in prior art and electrolytic process separation of lead and bismuth, the object of the invention is to be to provide a kind of technique that goes out high purity bismuth by simple process continuous separating-purifying from lead bismuth alloy, this technique low cost, less energy-consumption, environmental protection, meet demand of industrial production.
The invention provides a kind of from lead bismuth alloy the technique of separating-purifying bismuth, this technique is to adopt vacuum distilling furnace system to carry out continous vacuum fractionation by distillation purification bismuth to lead bismuth alloy, described vacuum distilling furnace system comprises smelting furnace, siphon groove and vacuum distillation furnace, and vacuum distillation furnace comprises body of heater and inner bag, smelting furnace bottom is provided with discharge nozzle, and discharge nozzle one end is stretched in siphon groove, between siphon groove and vacuum distillation furnace, is provided with siphon pipe, and siphon groove bottom is stretched in siphon pipe one end, and the other end stretches into vacuum distilling furnace body inner upper end, the top of described inner bag is provided with metal reservoir, and the middle part in inner bag is provided with multilayer distillation tray, and lower floor distillation tray bottom is provided with groove, and bottom portion of groove is connected with going out of body of heater outside plumbous collector by pipeline, and the bottom in inner bag is provided with out bismuth pipe, while carrying out lead bismuth alloy fractionation by distillation purification bismuth, open vacuum pump and heating system, make vacuum distilling furnace interior be negative pressure state, the temperature of smelting furnace and siphon groove is elevated to 500～550 ℃, and the temperature of distillation tray is elevated to 1550～1600 ℃, now, lead bismuth alloy is sent into continuously in smelting furnace body of heater and melted, fusing gained molten metal flows in siphon groove, under the low pressure effect of molten metal in siphon groove in vacuum distillation furnace, by siphon pipe, be siphoned into the metal reservoir that injects inner bag top in vacuum distillation furnace, entering inner bag inside flows on the distillation tray of upper strata again, and successively to lower floor's distillation tray, flow from upper strata distillation tray, maintain vacuum distillation furnace internal vacuum < 8Pa, bismuth seethes with excitement and evaporates in each layer of distillation tray, after bismuth vapour is encountered inner bag inwall, condensation is gathered into liquid state, by the bismuth pipe that goes out of inner bag bottom, discharge collection in time, and comprise that plumbous high boiling point alloyed metal liquid is along the distillation tray dirty groove that enters into distillation tray bottom successively always, by bottom portion of groove pipeline, entering plumbous collector again collects, complete vacuum distilling from lead bismuth alloy and isolate pure bismuth.
Of the present invention from lead bismuth alloy the technique of separating-purifying bismuth also comprise following preferred version:
In preferred scheme, the temperature of distillation tray is 1550～1575 ℃; Most preferably be 1550 ℃.
In preferred scheme, the temperature of smelting furnace and siphon groove maintains 520～540 ℃; Most preferably be 520 ℃, to keep the liquid phase of the best of molten metal.
In preferred scheme, vacuum distillation furnace bottom of furnace body is provided with upflow tube; Upflow tube can be discharged the excessive molten metal of vacuum distilling furnace interior in time, protection body of heater.
In preferred scheme, metal reservoir bottom is provided with aperture and inner bag internal communication.
In preferred scheme, when the metal reservoir at inner bag top in, during molten metal overfill, overflow to the bottom in body of heater, from upflow tube discharge body of heater.
In preferred scheme, go out bismuth pipe at the outside vacuum collection device that connects of vacuum distillation furnace.
In preferred scheme, side wall of inner is provided with vacuum-pumping tube, and vacuum-pumping tube is connected with the vacuum pump of body of heater outside.
In preferred scheme, distillation tray is set to 3～8 layers, most preferably is 3～5 layers.
Beneficial effect of the present invention: the present invention designs a kind of by vacuum distillation furnace system and device first, and in conjunction with this device, design the technique of the high purity metal bismuth of purifying out by vacuum distilling separation from plumbous bismuth metal.The relative prior art of technique of the present invention has the following advantages: 1, simple for process, can produce continuously; 2, still less, energy consumption is low, with low cost for equipment and input; 3, environmental pollution is little, almost there is no waste gas, does not produce waste water, and waste residue is few; 3, good separating effect, isolated bismuth purity >=99.9%, without follow-up refining processing, residual without bismuth in the metallic lead that separation obtains.
Accompanying drawing explanation
[Fig. 1] is lead content and distillation temperature graph of relation in bismuth of the present invention.
[Fig. 2] is vacuum distillation furnace system device structure diagram; 1 is smelting furnace, and 2 is refractory brick, and 3 is nichrome wire, and 4 is entrance of cooling water, 5 is base, and 6 is stirring rake, and 7 is cooling water outlet, and 8 is discharge nozzle valve, 9 is discharge nozzle, and 10 is siphon groove, and 11 is siphon pipe, and 12 is siphon pipe valve, 13 is vacuum distilling furnace body, and 14 is vacuum distilling furnace internal-lining, and 15 is distillation tray, and 16 is electrode, 17 is upflow tube valve, and 18 for going out bismuth tube valve, and 19 is upflow tube, 20 for going out bismuth pipe, and 21 is plumbous collector, and 22 is vacuum-pumping tube; 23 is groove, and 24 is metal reservoir.
Embodiment
Following examples are intended to further illustrate content of the present invention, rather than limit the scope of the invention.
Embodiment 1
The lead bismuth alloy adopting derives from smeltery, Jiangxi, and wherein Fe, Cu, As and Cd content are below 0.3wt%, and Sb content is below 0.5wt%, and Ag content is in 2wt%.Adopt atomic absorption spectrometry to detect; Detecting instrument: atomic absorption spectrophotometer (hydrogeneous compound producer), AA320N.
With reference to the vacuum distilling tripping device system of accompanying drawing 2, carry out lead bismuth alloy fractionation by distillation purification bismuth.Described vacuum distilling furnace system comprises smelting furnace, siphon groove and vacuum distillation furnace, and vacuum distillation furnace comprises body of heater and inner bag; Smelting furnace bottom is provided with discharge nozzle, and the discharge nozzle the other end stretches in siphon groove, between siphon groove and vacuum distillation furnace, is provided with siphon pipe, and siphon groove bottom is stretched in siphon pipe one end, and the other end stretches into vacuum distilling furnace body inner upper end; The top of described inner bag is provided with metal reservoir, middle part in inner bag is provided with 3～5 layers of distillation tray, lower floor's distillation tray bottom is provided with groove, bottom portion of groove is connected with going out of body of heater outside plumbous collector by pipeline, bottom in inner bag is provided with out bismuth pipe, goes out bismuth pipe at the outside vacuum collection device that connects of vacuum distillation furnace; Described vacuum distillation furnace bottom of furnace body is provided with upflow tube; Upflow tube can be discharged the excessive molten metal of vacuum distilling furnace interior in time, protection body of heater; Described metal reservoir bottom is provided with aperture and inner bag internal communication; In the metal reservoir at inner bag top, during molten metal overfill, overflow to the bottom in body of heater, from upflow tube, discharge body of heater; Described side wall of inner is provided with vacuum-pumping tube, and vacuum-pumping tube is connected with the vacuum pump of body of heater outside.
Material is sent in fusing body of heater by loading hopper with the speed of 5.2～5.8kg/h, open vacuum pump and heating system, when the vacuum tightness < of vacuum distilling furnace interior 20Pa, smelting furnace temperature is warmed up to 520 ℃, the temperature of siphon groove also maintains 520 ℃ simultaneously, the temperature of distillation tray is elevated to 1550 ℃, and lead bismuth alloy is melted in smelting furnace, and fusing gained molten metal flows in siphon groove, under the low pressure effect of molten metal in siphon groove in vacuum distillation furnace, by siphon pipe, be siphoned into the metal reservoir that injects inner bag top in vacuum distillation furnace, entering inner bag flows on the distillation tray of upper strata again, and successively to lower floor's distillation tray, flow from upper strata distillation tray, maintain vacuum distillation furnace internal vacuum < 8Pa, bismuth seethes with excitement and evaporates in each layer of distillation tray, after bismuth vapour is encountered inner bag inwall, condensation is gathered into liquid state, in time the bismuth pipe that goes out by inner bag bottom discharges out of the furnace and collects by vacuum collection device, and comprise that plumbous high boiling point alloyed metal liquid is along the distillation tray dirty groove that enters into distillation tray bottom successively always, by bottom portion of groove pipeline, entering plumbous collector again collects, complete vacuum distilling from lead bismuth alloy and isolate pure bismuth.
Isolated bismuth metal and lead metal are detected to purity >=99.9% of bismuth; And in lead, can't detect bismuth metal.
The temperature of the interior distillation tray of vacuum distilling body of heater is repeated to above-mentioned experiment every 5 ℃ of values between 1550～1655 ℃, and the purity of bismuth metal and lead metal is detected, plumbous purity is substantially constant, and the purity of bismuth as shown in Figure 2, within the scope of 1550～1575 ℃, the purity of bismuth is all more than 99.9%; And in the scope of 1575～1600 ℃ the purity of bismuth all more than 99.8%; And within the scope of 1600～1625 ℃ between purity drop to 99.6～99.7% of bismuth; Illustrate that too high plumbous in bismuth product (the being mainly plumbous) impurity that causes of distillation temperature is significantly higher.
Experiment is also found in addition, and when temperature is during lower than 1550 ℃, it yields poorly, and has the hidden danger that causes the plumbous discharging mouth of pipe to block.And smelting temperature is too low, slowly even there is not melting phenomenon in the fusing of test interalloy; Smelting temperature is too high, causes part metals volatilization loss in raw material to fall, and has also increased energy consumption simultaneously.Take certain lead bismuth alloy raw material is example, wherein bismuth 63wt%, plumbous 35 wt%, gold and silver 1.7 wt%, below other metals 0.3 wt%, too low when smelting temperature, during lower than 325 ℃, because plumbous fusing point is 327.3 ℃, there will be part material not melt; Work as excess Temperature, during higher than 765 ℃, because part metals boiling point in raw material is lower, there will be part metals (as cadmium, potassium etc.) to vapor away, the too high corresponding energy consumption of simultaneous temperature has also increased.Therefore smelting temperature is unsuitable too high, also unsuitable too low, through test of many times, smelting temperature be 400～700 ℃ comparatively suitable, temperature at 475～525 ℃ for better.
Claims (10)
1. the technique of a separating-purifying bismuth from lead bismuth alloy, it is characterized in that, adopt vacuum distilling furnace system to carry out continous vacuum fractionation by distillation purification bismuth to lead bismuth alloy, described vacuum distilling furnace system comprises smelting furnace, siphon groove and vacuum distillation furnace, and vacuum distillation furnace comprises body of heater and inner bag, smelting furnace bottom is provided with discharge nozzle, and discharge nozzle one end is stretched in siphon groove, between siphon groove and vacuum distillation furnace, is provided with siphon pipe, and siphon groove bottom is stretched in siphon pipe one end, and the other end stretches into vacuum distilling furnace body inner upper end, the top of described inner bag is provided with metal reservoir, and the middle part in inner bag is provided with multilayer distillation tray, and lower floor distillation tray bottom is provided with groove, and bottom portion of groove is connected with going out of body of heater outside plumbous collector by pipeline, and the bottom in inner bag is provided with out bismuth pipe, while carrying out lead bismuth alloy fractionation by distillation purification bismuth, open vacuum pump and heating system, make vacuum distilling furnace interior be negative pressure state, the temperature of smelting furnace and siphon groove is elevated to 500～550 ℃, and the temperature of distillation tray is elevated to 1550～1600 ℃, now, lead bismuth alloy is sent into continuously in smelting furnace body of heater and melted, fusing gained molten metal flows in siphon groove, under the low pressure effect of molten metal in siphon groove in vacuum distillation furnace, by siphon pipe, be siphoned into the metal reservoir that injects inner bag top in vacuum distillation furnace, entering inner bag inside flows on the distillation tray of upper strata again, and successively to lower floor's distillation tray, flow from upper strata distillation tray, maintain vacuum distillation furnace internal vacuum < 8Pa, bismuth seethes with excitement and evaporates in each layer of distillation tray, after bismuth vapour is encountered inner bag inwall, condensation is gathered into liquid state, by the bismuth pipe that goes out of inner bag bottom, discharge collection in time, and comprise that plumbous high boiling point alloyed metal liquid is along the distillation tray dirty groove that enters into distillation tray bottom successively always, by bottom portion of groove pipeline, entering plumbous collector again collects, complete vacuum distilling from lead bismuth alloy and isolate pure bismuth.
2. technique as claimed in claim 1, is characterized in that, the temperature of described distillation tray is 1550～1575 ℃.
3. technique as claimed in claim 2, is characterized in that, the temperature of described distillation tray is 1550 ℃.
4. technique as claimed in claim 1, is characterized in that, described smelting furnace and the temperature of siphon groove maintain 520～540 ℃.
5. technique as claimed in claim 4, is characterized in that, described smelting furnace and the temperature of siphon groove maintain 520 ℃.
6. technique as claimed in claim 1, is characterized in that, described vacuum distillation furnace bottom of furnace body is provided with upflow tube.
7. technique as claimed in claim 1, is characterized in that, described metal reservoir bottom is provided with aperture and inner bag internal communication.
8. technique as claimed in claim 6, is characterized in that, in the metal reservoir at inner bag top, during molten metal overfill, overflows to the bottom in body of heater, from upflow tube, discharges body of heater.
9. technique as claimed in claim 1, is characterized in that, goes out bismuth pipe at the outside vacuum collection device that connects of vacuum distillation furnace.
10. technique as claimed in claim 1, is characterized in that, described side wall of inner is provided with vacuum-pumping tube, and vacuum-pumping tube is connected with the vacuum pump of body of heater outside.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779790A (en) * | 2016-04-12 | 2016-07-20 | 永兴佳盛有色金属再生利用有限责任公司 | Method for removing lead and purifying bismuth from lead-bismuth material through vacuum distillation |
| CN106048243A (en) * | 2016-08-11 | 2016-10-26 | 永兴佳盛有色金属再生利用有限责任公司 | Method for deep removal of bismuth through vacuum distillation of high-bismuth crude tin alloy |
| CN111504924A (en) * | 2020-04-23 | 2020-08-07 | 中国原子能科学研究院 | Method for removing lead and bismuth in lead-bismuth alloy and method for measuring cadmium in lead-bismuth alloy |
| CN115491509A (en) * | 2022-08-31 | 2022-12-20 | 永兴县鸿福金属有限公司 | Vacuum purification method for multi-stage extraction of refined bismuth |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
| CN102586627A (en) * | 2012-02-14 | 2012-07-18 | 蒙自矿冶有限责任公司 | Method for recovering bismuth from bismuth slag |
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2014
- 2014-07-31 CN CN201410373065.0A patent/CN104109766B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696469A (en) * | 2009-10-29 | 2010-04-21 | 昆明理工大学 | Method for separating multi-element alloy of lead, bismuth, gold, silver and copper |
| CN102586627A (en) * | 2012-02-14 | 2012-07-18 | 蒙自矿冶有限责任公司 | Method for recovering bismuth from bismuth slag |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779790A (en) * | 2016-04-12 | 2016-07-20 | 永兴佳盛有色金属再生利用有限责任公司 | Method for removing lead and purifying bismuth from lead-bismuth material through vacuum distillation |
| CN106048243A (en) * | 2016-08-11 | 2016-10-26 | 永兴佳盛有色金属再生利用有限责任公司 | Method for deep removal of bismuth through vacuum distillation of high-bismuth crude tin alloy |
| CN106048243B (en) * | 2016-08-11 | 2018-06-05 | 永兴佳盛环保科技有限责任公司 | A kind of method that high bismuth crude tin alloy vacuum distillation depth removes bismuth |
| CN111504924A (en) * | 2020-04-23 | 2020-08-07 | 中国原子能科学研究院 | Method for removing lead and bismuth in lead-bismuth alloy and method for measuring cadmium in lead-bismuth alloy |
| CN115491509A (en) * | 2022-08-31 | 2022-12-20 | 永兴县鸿福金属有限公司 | Vacuum purification method for multi-stage extraction of refined bismuth |
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