CN1224067A - Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver - Google Patents

Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver Download PDF

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Publication number
CN1224067A
CN1224067A CN 98107600 CN98107600A CN1224067A CN 1224067 A CN1224067 A CN 1224067A CN 98107600 CN98107600 CN 98107600 CN 98107600 A CN98107600 A CN 98107600A CN 1224067 A CN1224067 A CN 1224067A
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China
Prior art keywords
zinc
vacuum
hard
germanium
temperature
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CN 98107600
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Chinese (zh)
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CN1065919C (en
Inventor
戴永年
吴昆霖
杨斌
罗文洲
邓学广
李清湘
张国靖
杨部正
陈事农
吴昆华
曾志初
李金华
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Guangdong Shaoguan South Of Five Ridges Lead Zinc Group Co Ltd Shaoguan Smelter
Kunming University of Science and Technology
Original Assignee
Guangdong Shaoguan South Of Five Ridges Lead Zinc Group Co Ltd Shaoguan Smelter
Kunming University of Science and Technology
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Application filed by Guangdong Shaoguan South Of Five Ridges Lead Zinc Group Co Ltd Shaoguan Smelter, Kunming University of Science and Technology filed Critical Guangdong Shaoguan South Of Five Ridges Lead Zinc Group Co Ltd Shaoguan Smelter
Priority to CN98107600A priority Critical patent/CN1065919C/en
Publication of CN1224067A publication Critical patent/CN1224067A/en
Application granted granted Critical
Publication of CN1065919C publication Critical patent/CN1065919C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

A vacuum distillation process for extracting zinc from hard zinc and enriching Ge, In and Ag includes evaporating zinc at 900-960 deg.C and 1-2 mmHg of vacuum degree for less than 16 hr and condensing at 460 deg.C or more in vacuum furnace to obtain zinc ingot, coarse lead and Ge slags, loading coarse lead in vacuum furnace to separate coarse lead from Ge slags, and recovering Ge, In and Ag from Ge slags. Its advantages are short process and high stability and safety.

Description

Vacuum distillating hard-zinc is carried zinc and enriched germanium indium silver
Vacuum distillating hard-zinc carries zinc and enriched germanium indium silver is a kind of non-ferrous metal pyrometallurgical smelting process.
Hard zinc is a kind of byproduct of output in the zinc refining process, and its major ingredient dezincifies, plumbous outer also have germanium, indium, and multiple valuable metals such as silver, tin, copper have the value of very high comprehensively recovering valuable metal.The technology of this hard zinc of known processing is with muffle-electric furnace production technique, the hard zinc of different components is used every sunken reverberatory furnace or induction furnace and is handled, obtain zinc powder, lead bullion and cadmia, lead bullion obtains lead bullion and germanium scarp through remelting again, the germanium scarp is handled through electric furnace and is further isolated zinc oxide, lead bullion and high arsenic germanium scarp, lead bullion send blast furnace to handle, and the germanium scarp is sent back to and received germanium, indium, silver.It is low that this muffle-the electric furnace production technique exists the germanium indium recovery, and other valuable metals are difficult for reclaiming, electric furnace washes away uneasy congruent problem.The applicant is on the basis of 97101388 patent application at application number, further replenishment of process flow process, equipment and processing condition, and 2.5 tons of horizontal vacuum furnaces have successfully been designed, it is reasonable that the structure of stove more becomes, taken measures to guarantee the vacuum tightness of stove, improved the heat supply of stove, the extension zinc that has solved condenser is tied the problem of waiting indefinitely, make the industrial applicability of this technology become reality, and reliable, stable.The objective of the invention is to adopt vacuum tightness, temperature in the horizontal vacuum furnace control stove, and tap to tap time, make hard zinc one step dezincify and enriched germanium, cigarette, silver.
Technology contents of the present invention is as follows:
One, technical process and processing condition
Technical process as shown in Figure 1, hard zinc through the batching entrucking.Push in the vacuum oven, vacuumize and heat up, dezincify obtains zinc ingot metal, lead bullion and germanium slag in steaming empty stove.The germanium slag is sent back to and is received germanium, cigarette, silver, lead bullion and reenter vacuum oven and smelt (or adding the alkali slag making), isolates plumbous and germanium slag once more, and the germanium slag is sent receipts germanium, cigarette, silver back to, and lead bullion returns blast furnace.
The composition scope of hard zinc as shown in Figure 2.
Technology condition
1, steams 900-960 ℃ of zinc temperature;
2, optimal vacuum pressure 1 one 2mmHg;
3, total tap to tap time was less than 16 hours;
4, the processing power 2.5 tons/stove day of vacuum oven;
5, the condensing chamber temperature is greater than 460 ℃;
6, best drop temperature is 750 ℃.
Two, equipment
Used vacuum oven is formed structure shown in Figure of description 3.
Mainly by putting zinc mouth 1, the bright water jacket 2 of stove, extraction pipe 3, condensation wall 4, refractory materials masonry 5, thermometric flange 6, electrode 7 adds trolley 8 and forms.
The solid input and output material is by adding the turnover of trolley loading material.Utility appliance also has input and output material windlass, vacuum pump, magnetic voltage regulator, pressure regulation to hand over depressor, transformer, silicon controlled rectifier voltage adjustment etc.
Several technical barriers down below in the equipment design process, having solved.
1, adds section's dolly Steel Concrete ramming, the interior reinforcement plate of dolly, dolly medullary ray and vacuum oven central lines when smelting;
2, all sealing members of vacuum oven adopt the viton bar, make equipment obtain excellent sealing performance;
3, water-cooled tube is the open channel discharging, make to the steaming of steaming zinc in the zinc process put, the monitoring of the flow of degree of condensation and water coolant is more convenient;
4, strengthen the air switch rated value of low-voltage distribution cabinet, adopt pressure regulation friendship depressor and cancelled temperature automatically controlled function.Distribution and control stability and reliability have partly been strengthened;
5, horizontal vacuum furnace requirement graphite electric heating element is not consume and the least possible consumption, the stress cracking of eliminating electrode by the installation and the production standard of strictness, baker system by strictness reduces the oxidation of telegram to reduce the corrosion of high temperature water gas to telegram by the low temperature discharging.Reaching increases electrode life, reduces the purpose that telegram consumes.
6, the two walls with condenser make single wall into, and reduce the water pipe quantity of condenser, have guaranteed the temperature of liquid zinc in the condenser, reduce the divinatory symbol quantity of slag of condenser wall, prolong cleaning period.
Make vacuum oven not only can satisfy processing requirement by above-mentioned improvement, and reliable, stable.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the composition scope of raw material hard zinc;
Fig. 3 is the composition structure sectional view of vacuum oven, and 1 is to put the zinc mouth among the figure, the 2nd, and the furnace shell water jacket, the 3rd, extraction pipe, the 4th, the condensation wall, the 5th, the refractory materials masonry, the 6th, the thermometric flange, the 7th, electrode, the 8th, add trolley;
Fig. 4 is the list of main equipment that 2.5T/ stove day vacuum oven is handled hard zinc;
Fig. 5 is the technico-economical comparison that 2.5T/ stove day vacuum oven is handled hard zinc;
Fig. 6 is the cost structure composition table that 2.5T/ stove day vacuum oven is handled hard zinc;
Fig. 7 is the product composition table that 2.5T/ stove day vacuum oven is handled hard zinc.
The advantage that has of the present invention compared with prior art
1, collect the dezincify concentration of valuable metals in a stove, flow process is short, and floor space is little, and equipment is simple, Reduced investment, production cost is low;
2, adopt horizontal vacuum furnace. The solid input and output material, material loading trolley does solid through armored concrete, and adds Reinforcement plate has prevented from oozing plumbous phenomenon, and dolly is in position, concentric garden with body of heater, has improved steaming zinc efficient;
3, the seal of vacuum drying oven adopts the fluorubber bar, makes equipment obtain good sealing, has improved The thermal efficiency has reduced environmental pollution;
4, condenser is single wall, and condensate pipe is received with open channel row, so that the degree of being condensed into of zinc and cooling water Traffic monitoring more convenient.
Embodiment
Use the 2.5T/ stove, day horizontal vacuum furnace is handled the byproduct-hard zinc of output in certain smeltery's zinc refining process, and its major ingredient is seen Figure of description 2 (it is plumbous tower hard zinc of this factory and 3# tower hard zinc).
1, technical process is as shown in Figure of description 1 is
2, main technique condition
Steam 900-950 ℃ of zinc temperature
Vacuum tightness 1-2mmHg
15 hours tap to tap time
About 500 ℃ of condensing chamber temperature
Go out 750 ℃ of car temperature
3, major equipment
1 of horizontal vacuum furnace, structure is formed as shown in Figure 3 in specification: φ * 4265
Add 2 of trolleys, load-carrying: 2.5 tons
1 in input and output material windlass, power of motor: 5KW
2 in vacuum pump, model: 2x-15,2x-30
1 of magnetic voltage regulator, model: TSH-315/0.5
1 of powerstat, model: TDGC2J-5/0.5
1 of transformer, model: BK-4200
Silicon controlled rectifier voltage is adjusted 1, model ZK-1
Technico-economical comparison in the smelting process is seen shown in Figure 5, and Fig. 6 is the cost structure table of present embodiment, and the smelting result obtains product composition table as shown in Figure 7.

Claims (2)

1, a kind of vacuum distillating hard-zinc is carried zinc and the enrichment germanium, indium and silver is a kind of pyrometallurgy method, this method is to place vacuum oven to smelt hard zinc, the solid input and output material, temperature in the control stove, vacuum tightness, distillation time and condensing temperature make zinc distill output germanium slag from raw material, it is characterized in that the technical qualification of controlling in the vacuum oven are: steam 900~960 ℃ of zinc temperature, optimal vacuum pressure 1-2mmHg, distillation time; The cooling room temperature is greater than 460 ℃; 750 ℃ of best discharging (car) temperature.
2, a kind of vacuum distillating hard-zinc is carried the equipment of zinc and enrichment germanium, indium and silver, be a kind of horizontal vacuum furnace, it is by putting zinc mouth 1, furnace shell water jacket 2, extraction pipe 3, condensation wall 4, refractory materials masonry 5, thermometric flange 6, telegram 7, add trolley 8, forming and it is characterized in that:
1) add trolley Steel Concrete ramming, dolly medullary ray and vacuum oven central lines during smelting are pulled in lacing wire in the dolly;
2) all sealing members of vacuum oven adopt the viton bar
3) water-cooled tube is the open channel discharging;
4) adopt powerstat
5) condenser is single wall.
CN98107600A 1998-04-24 1998-04-24 Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver Expired - Fee Related CN1065919C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN98107600A CN1065919C (en) 1998-04-24 1998-04-24 Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN98107600A CN1065919C (en) 1998-04-24 1998-04-24 Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver

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CN1224067A true CN1224067A (en) 1999-07-28
CN1065919C CN1065919C (en) 2001-05-16

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2813614A1 (en) * 2000-09-07 2002-03-08 Metaleurop Sa PROCESS FOR RECOVERING METALLIC ELEMENTS FROM ZINCIFEROUS RAW MATERIALS
CN102277504A (en) * 2011-08-19 2011-12-14 赵志强 Process for extracting zinc and indium by rectifying hard zinc under constant pressure
CN108642296A (en) * 2018-07-13 2018-10-12 昆明理工大学 A method of lead and zinc are separated and recovered by hard lead

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2288299C2 (en) * 2001-08-14 2006-11-27 Мэгпауэр Системз, Инк. Additives inhibiting liberation of hydrogen at electrolytic separation of zinc
CN101565779B (en) * 2009-05-18 2011-06-08 葫芦岛锌业股份有限公司 Method for producing zinc powder and reclaiming scattered metals indium and germanium by distilling aluminum hard zinc in vacuum

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1023818C (en) * 1991-03-19 1994-02-16 昆明工学院 Vacuum distillation zinc extraction method of hot galvanizing residue
CN1162649A (en) * 1997-02-28 1997-10-22 昆明理工大学 Method for enriching noble metals and extracting zinc by vacuum vaporization

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2813614A1 (en) * 2000-09-07 2002-03-08 Metaleurop Sa PROCESS FOR RECOVERING METALLIC ELEMENTS FROM ZINCIFEROUS RAW MATERIALS
WO2002020858A1 (en) * 2000-09-07 2002-03-14 Metaleurop S.A. Method for recuperating metal elements from zinc-bearing raw materials using molten lead
CN102277504A (en) * 2011-08-19 2011-12-14 赵志强 Process for extracting zinc and indium by rectifying hard zinc under constant pressure
CN102277504B (en) * 2011-08-19 2016-02-10 赵志强 Hard zinc atmospheric distillation extracts zinc, indium technique
CN108642296A (en) * 2018-07-13 2018-10-12 昆明理工大学 A method of lead and zinc are separated and recovered by hard lead
CN108642296B (en) * 2018-07-13 2020-04-07 昆明理工大学 Method for separating and recovering lead and zinc from lead-zinc alloy

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