CN1051202A - Separation of zn-cd alloy by vacuum distillation - Google Patents

Separation of zn-cd alloy by vacuum distillation Download PDF

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Publication number
CN1051202A
CN1051202A CN 89108164 CN89108164A CN1051202A CN 1051202 A CN1051202 A CN 1051202A CN 89108164 CN89108164 CN 89108164 CN 89108164 A CN89108164 A CN 89108164A CN 1051202 A CN1051202 A CN 1051202A
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China
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vacuum
alloy
cadmium
zinc
distillation
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CN 89108164
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CN1020382C (en
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戴永年
李淑兰
邓琴芳
张本明
施恩潭
黎锡辉
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Publication of CN1020382C publication Critical patent/CN1020382C/en
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Abstract

Separation of Zn-Cd alloy by vacuum distillation is a kind of vacuum metallurgy technology.Vacuum tightness 10~30 torrs in the Zn-Cd alloy adding vacuum oven with molten state, in the control stove, 19~25 grades of technical qualification such as feed rate of 690~720 ℃ of distillation tray progression of furnace temperature, make zinc and cadmium divide evaporation successively, and collect, make zinc and cadmium to obtain separating purification respectively.This method facility investment is few, and metal recovery rate height, workshop floor space are little, initial cost has been eliminated the pollution to environment not quite, basically.

Description

Separation of Zn-Cd alloy by vacuum distillation
It is a kind of vacuum metallurgy technology that Zn-Cd alloy by vacuum distillation separates.
At present, handle Zn-Cd alloy both at home and abroad and adopt the atmospheric distillation method, the zinc cadmium can be separated into metallic zinc and cadmium metal.But energy consumption is big, the huge investment of equipment is also big for this method processing temperature height (1050~1200 ℃), also needs expensive carbofrax material.
The applicant Ceng Jin is used successfully in terne metal to the vacuum distilling method and separates the separation of bismuth-silver-zinc-containing shell etc.In the patent No. is 87104574 patent of invention, the applicant discloses a kind of fire refining of crude lead technology, its be utilize about 1100 ℃ of the temperature of vacuum metallurgy, control vacuum oven, because plumbous bismuth and silver-colored isolating purpose are come out, reached to the vapour pressure of lead and bismuth greater than silver by preferential evaporation.At application number is that 88104601.9 file then is to utilize vacuum technique, and 900~1120 ℃ of vacuum tightnesss of temperature are to charge into argon, nitrogen rare gas element zinc and bismuth evaporation in 26~52 torr stoves in the control stove, and rich silver alloys remains in and reaches separating of zinc bismuth and silver in the evaporating pan.
The application's purpose is to want to make zinc and cadmium divide successively evaporation, enrichment by technical qualification such as temperature, vacuum tightness in the vacuum metallurgy technology control stove equally, and the purpose that reaches separation, purifies.
Main contents of the present invention are as follows:
One, theoretical foundation
Because zinc, cadmium boiling point and steam are pressed with than big-difference, the zinc of pure state and the vapor pressure ratio of cadmium be P in 227~627 ℃ of temperature ranges O Cd/ P 0 Zn=43.9~6.7 is the cadmium preferential volatilization, but both ratios all with the rising of temperature successively decrease, because zinc also have volatility so, so the selection of distillation temperature should consider metallic zinc volatilization and with the isolating effect of cadmium.Distillation temperature hangs down, adopts simultaneously multistage distillation to separate, and zinc separates comparatively thorough with cadmium.
Two, furnace construction and processing condition
1. furnace type structure as shown in Figure 1.Mainly by peep hole (1), bell (2), shaft (3), insulation plate (4), go out cadmium and chew (5), go out cadmium pipe (6), distillation tray (7), electricity post (8), go out zinc and chew (9), go out zinc pipe (10), current conducting rod (11), (12) are chewed in charging, and feed-pipe composition bodies of heater such as (13) all is welded with common steel tube.
Dress graphite system heating member (electric post) places in the distillation tray pipe core in the stove.Allow radiant heat directly pass in the distillation tray to improve thermo-efficiency.
The enclosed distillation tray with common graphite make, each all has an overflow port, overflow liquid metal also to be both the passage of gas on trying to get to the heart of a matter.A plurality of dishes are overlapped into post, the center is passed electric post, is placed on the furnace bottom support, dish with coil between airtight slit, respectively coil overflow port and interlace 180 ° and arrange, purpose is to prolong gas, the time that liquid stops in stove, pass process to promote heat to pass, be beneficial to the quality and the output that improve product with matter.
Distillation tray has 1 of the insulation plate of iron plate system outward, with the concentric(al) circles tubular place between dish post and the stove inwall, block resistance is to the thermal radiation of furnace wall, the heat that the minimizing water coolant is taken away can make and rise to high temperature in the stove fast.
Electrical equipment partly mainly partly is made up of main power circuit and pair circuit two.Main power circuit is by one of dry type transformer of heating, vacuum stove, and one of silicon-controlled rectifier is sent into the direct current heating in stove.Pay circuit one for the input and output material system melting charge and the insulation electricity consumption, for the temperature of keeping input and output material pot and pipe is certain, respectively with voltate regulator control power input to keep homo(io)thermism.Two for finding time and measuring, use one in rotating-expressing type vacuum pump, measures the following wheat formula vacuumometer mensuration of using of 1 torr more than vacuum tightness 1 torr with V shape pressure warning unit.Aforesaid device interface chart as shown in Figure 2.
2 technical qualification and schedule of operation
The ready back that meets the requirements all is installed inside and outside the stove, with charging, go out zinc and go out three pipes of cadmium to imbed respectively in three mouthfuls of pots, allow melt cooled and solidified in the pot, can reach about 10 torrs and get final product blow-on the total system vacuum tightness of finding time to hunt leak.
At this moment, termination of pumping, applying argon gas in the intensification of all switching on of three pipes and three mouthfuls of pots, when treating the material local melting in the pot, is connected main circuit power to normal atmosphere in stove, and furnace temperature is evenly risen, and the temperature with three pipes and three mouthfuls of pots is adjusted to preset value simultaneously.When furnace temperature reaches 690~720 ℃, stablized again 0.5 hour, and closed argon gas, the vacuum tightness of finding time 10~30 torrs, start hydraulicefficiency elevation structure and adjust charging pot liquid level by its charging.Raw alloy composition Cd%+Zn%>99%, containing cadmium can be surplus percentum to percent 90, the very little raw material of other impurity flows in the feed tray at king-post middle part, zinc and cadmium are pressed the size of vapour pressure separately, evaporation to some extent, the steam of rich cadmium passes overflow port and enters the last layer distillation tray and contact and the part condensation with its liquid of going up existence, be rich in zinc in the phlegma, flow in the process of following one deck dish again, contact and partly gasification with the steam that rises, tell again than liquid and contain the richer steam of cadmium, promptly partly volatile cadmium changes gas phase over to from liquid phase gradually, just may get pure zinc through flowing into undermost liquid behind the several layers dish.Steam wherein high boiling zinc in the process that enters the last layer distillation tray can successively be condensed and enter liquid phase, in the steam of rising just gradually enrichment lower boiling cadmium, after it is through several layers dish, rise to, just obtain purer cadmium.
Pure zinc and pure cadmium enter zinc pot and cadmium pot by zinc pipe and cadmium pipe respectively, and the chute through pot flows out ingot casting again.After this continuously feeding, discharging continuously are with input speed control discharging speed.
All stop charging during improper or normal blowing out earlier; when back cut-out main circuit power is reduced to 300 ℃ by furnace temperature; termination of pumping, applying argon gas are gone into stove, and at this moment the liquid level of three mouthfuls of pots all will rise, prepare the horizontal pipe of discharging to three respectively of ingot and imbed and stop discharging when liquid level reaches the degree of depth of preparatory stage, cut off and pay a circuit power, close the argon gas blowing out when furnace temperature is reduced to 50 ℃.
For the running period of improving stove, prevent that line clogging from improving quality product, also can take following measure:
1. make of carbon tube that charging is chewed in case flash, causes short circuit current to furnace bottom and blowing out.
2. the graphite charging is chewed around last resistance wire heating, is prevented that material from freezing near proceeding to herein.
Feed and exhaust tube stretch in the stove one section all with asbestos wrapping insulation, prevent that material from freezing in this section.
4. elder generation's applying argon gas protection when heating up cooling, avoid burning, generate dystectic slag and to influence pipeline unimpeded.
5. strict control tube pot temperature suitably reduces the vacuum tightness charging, to prevent material spray.
6. increase distillation progression, improve quality product
Three, embodiment:
Material composition: Cd 11.52%, Zn 88.34%
Average feed rate: 9.37 kilograms/hour
Vacuum tightness 15 torrs
Furnace temperature: 700 ℃
Distillation progression: 20 grades
The output pure cadmium contains Cd 99.94%, and crude zinc contains Zn 96.13% and contains Cd 3.83%.
The present invention compares with atmospheric distillation, and to have processing charges low, the metal recovery rate height, and equipment investment is few, the advantages such as long-pending little capital expenditure is few are taken up an area in the workshop.

Claims (4)

1, a kind of Zn-Cd alloy vacuum separation method, the alloy of molten state is added in the vacuum oven, vacuum tightness, furnace temperature distillation tray progression and feed rate etc. in the control stove, each composition of alloy is evaporated respectively and collects, it is characterized in that: vacuum tightness 10~30 torrs in the control stove, 690~720 ℃ of furnace temperature, 19 to 25 grades of evaporating pan progression, material composition Cd%+Zn>99%.
2, vacuum separation method as claimed in claim 1 is characterized in that charging is chewed with carbon tube to make.
As claim 1,2 described vacuum separation methods, it is characterized in that 3, the graphite charging is chewed around last resistance wire heating.
4, as claim 1,2,3 described vacuum separation methods, it is characterized in that the material composition of handling is Cd11.52%, Zn88.32%.
CN 89108164 1989-10-21 1989-10-21 Separation of zn-cd alloy by vacuum distillation Expired - Fee Related CN1020382C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 89108164 CN1020382C (en) 1989-10-21 1989-10-21 Separation of zn-cd alloy by vacuum distillation

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Application Number Priority Date Filing Date Title
CN 89108164 CN1020382C (en) 1989-10-21 1989-10-21 Separation of zn-cd alloy by vacuum distillation

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CN1051202A true CN1051202A (en) 1991-05-08
CN1020382C CN1020382C (en) 1993-04-28

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942564A (en) * 2010-08-21 2011-01-12 赵志强 Process for producing pure cadmium by continuous reduction and distillation of zinc cadmium slag and sponge cadmium
CN102517455A (en) * 2011-12-29 2012-06-27 株洲冶炼集团股份有限公司 Method for recovering cadmium from copper cadmium residues
CN103184349A (en) * 2011-12-29 2013-07-03 广东先导稀材股份有限公司 High purity zinc preparation device and method
CN104263935A (en) * 2014-09-05 2015-01-07 昆明理工大学 Method for improving vacuum distillation separation efficiency of high-cadmium zinc

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942564A (en) * 2010-08-21 2011-01-12 赵志强 Process for producing pure cadmium by continuous reduction and distillation of zinc cadmium slag and sponge cadmium
CN101942564B (en) * 2010-08-21 2013-09-25 赵志强 Process for producing pure cadmium by continuous reduction and distillation of zinc cadmium slag and sponge cadmium
CN102517455A (en) * 2011-12-29 2012-06-27 株洲冶炼集团股份有限公司 Method for recovering cadmium from copper cadmium residues
CN103184349A (en) * 2011-12-29 2013-07-03 广东先导稀材股份有限公司 High purity zinc preparation device and method
CN103184349B (en) * 2011-12-29 2014-07-23 广东先导稀材股份有限公司 High purity zinc preparation device and method
CN104263935A (en) * 2014-09-05 2015-01-07 昆明理工大学 Method for improving vacuum distillation separation efficiency of high-cadmium zinc

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CN1020382C (en) 1993-04-28

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