CN105603224B - A kind of leaded discarded object configures the smelting process of lead-antimony alloy - Google Patents
A kind of leaded discarded object configures the smelting process of lead-antimony alloy Download PDFInfo
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- CN105603224B CN105603224B CN201510985709.6A CN201510985709A CN105603224B CN 105603224 B CN105603224 B CN 105603224B CN 201510985709 A CN201510985709 A CN 201510985709A CN 105603224 B CN105603224 B CN 105603224B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C11/00—Alloys based on lead
- C22C11/08—Alloys based on lead with antimony or bismuth as the next major constituent
- C22C11/10—Alloys based on lead with antimony or bismuth as the next major constituent with tin
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Abstract
The present invention relates to non-ferrous metal metallurgy method and technology field, and in particular to a kind of leaded discarded object configures the smelting process of lead-antimony alloy, and it includes following steps, a, leaded discarded object is filled into pot, melts it completely at 327 DEG C or so；B, it is warming up to 380 ± 20 DEG C, adds rosin, be put into mixer stirring, lead skim is changed into chemically examining the content of copper when black powder or fine particle shape, and drags for golden scum silica frost；C, be warming up to 420 ± 20 DEG C, the mixture of ferrous disulfide and Cosan added by a certain percentage, treats that scum silica frost becomes loose, do not lumpd, darkly toner foam or during fine particle shape chemical examination copper and sulphur content, and drag for golden scum silica frost；D, it is warming up to 500 ± 20 DEG C, adds sodium hydroxide and sodium nitrate, each component content is chemically examined after stirring a period of time；E, the content of each composition and the component requirements of alloy according to gained in previous step add star antimony, pure tin, pure arsenic, pure selenium in order.
Description
Technical field
The present invention relates to non-ferrous metal metallurgy method and technology field, more particularly to input cost is low, safety and environmental protection system
A kind of leaded discarded object that number is high, production efficiency is high configures the smelting process of lead-antimony alloy.
Background technology
With reviver industrial expansion, the recovery utilization rate more and more higher of waste and old lead acid accumulator is for a long time, industrial
On sulphur slag making copper removal, a kind of Chinese invention patent application prospectus " lead bullion fire are added using red phosphorus copper removal or low temperature always
The first step refining process of method "（Patent No. CN103667737A）, including following steps：1st, several lead bullion and anode scrap collocation are filled
Pot, is once filled, lid dust collection cover；2nd, heating fusing, 360 DEG C or so of temperature control, pressure slag, pressure slag stone roller are hung when having a small amount of viscous lead
Enter the mixer with dust collection cover；3rd, flux will be prepared（Wood sawdust, sulphur, piece alkali, sodium carbonate, sodium nitrate）By a certain amount of artificial general
Slow unrestrained added with scoop is stirred in pot；4th, 1~2 hour to be mixed, scum silica frost is waited（Sulfur residue）Become loose, do not lump, be in
Powdery or granular during brownish black, represents that reaction is reached home, then stops stirring；5th, drag for slag and scum silica frost poured into iron plate sample examination,
Enter reverberatory furnace processing；6th, lead liquid will after lead liquid sample examination, be scooped to casting mold pot, but this lead bullion pyrogenic process just deposit by step refining process
Under cryogenic conditions danger coefficient height, lead skim inferior separating effect, length duty cycle, employee work intensity is big and copper is easily returned
It is molten, the shortcomings of energy consumption cost is high, hinder the raising of production efficiency.
The content of the invention
The present invention is directed to energy consumption cost height, the technical problem of low production efficiency that prior art is present, and provides a kind of throwing
Enter the smelting process that a kind of leaded discarded object that cost is low, safety and environmental protection coefficient is high, production efficiency is high configures lead-antimony alloy.
The technical solution adopted in the present invention is：
A kind of leaded discarded object configures the smelting process of lead-antimony alloy, and it includes following steps：
A, leaded discarded object filled into pot, once fill it up with, be capped pot cover, by temperature control at 327 DEG C or so to leaded discarded
Thing is completely melt；
B, reduction slag making：380 ± 20 DEG C are continuously heating to, in terms of the weight of leaded discarded object, 0.007% rosin is added
Enter in pot, be put into mixer and stirred 15-30 minutes with 20-25Hz frequency, promote lead skim to be changed into black powder or fine particle
Shape, by mixer FREQUENCY CONTROL in 10-15Hz, takes first sample to chemically examine the content of copper with direct-reading spectrometer, drags for most scum silica frost；
C, copper removal：420 ± 20 DEG C are continuously heating to, mixer FREQUENCY CONTROL is stirred in 35Hz, pressed（Sulphur：Two sulphur
Change iron=2:1）：Copper=1:1 amount adds the mixture of ferrous disulfide and Cosan, stirs 15-30 minutes, treats that scum silica frost becomes thin
Pine, do not lump, darkly toner foam or fine particle shape represent that reaction reaches terminal, by mixer FREQUENCY CONTROL in 20Hz, sampling
The content of copper and sulphur is chemically examined with direct-reading spectrometer, most scum silica frost is dragged for；
D, stokehold refining：500 ± 20 DEG C are continuously heating to, in terms of the weight of leaded discarded object, by 0.04% hydroxide
Sodium and 0.02% sodium nitrate are added in pot, are stirred 1.5-2 hour, and sampling is with direct-reading spectrometer chemical examination antimony, tin, arsenic, selenium
Content, drags for most scum silica frost；
E, alloy configuration：520 ± 20 DEG C are continuously heating to, with the content and lead-antimony alloy of the antimony detected in step d
The star antimony addition that mathematic interpolation between the component requirements content of antimony is drawn adds star antimony, and the FREQUENCY CONTROL of mixer is existed
Stir 10-15 minutes, by temperature control at 480 ± 20 DEG C, closed with the content of the tin detected in step d and lead antimony within 20Hz
The pure tin addition that mathematic interpolation in gold between the component requirements content of tin is drawn adds pure tin, by the FREQUENCY CONTROL of mixer
Stir 10-15 minute, wanted with the composition of arsenic in the arsenic detected in step d, the content of selenium and lead-antimony alloy, selenium within 20Hz
Pure arsenic, the pure arsenic of pure selenium addition addition, pure selenium that the mathematic interpolation between content is drawn are asked, the FREQUENCY CONTROL of mixer is existed
25Hz or so is stirred 10-15 minutes, and the content of each composition is chemically examined in sampling with direct-reading spectrometer, is opened lead pump and is started ingot casting.
The content for the copper chemically examined in described step b is not less than 0.003%.
The content for the copper chemically examined in described step c is not more than 0.003%, and the content of sulphur is not more than 0.01%.
Sodium hydroxide is first added in described step d, sodium nitrate is added.
Pure arsenic is first added in described step e, pure selenium is added.
The content for the copper chemically examined in described step b, which is not more than 0.003%, can directly carry out step d operation.
Repeat step c is needed not less than 0.003% for the content for the copper chemically examined in described step c until the content of copper is not more than
0.003%.
Lead-antimony alloy tailing remaining in pot after the completion of ingot casting can be mixed with leaded discarded object in described step e
The raw material smelted as next batch.
Reaction equation during the inventive method copper removal is：
The beneficial effects of the present invention are：
1. ferrous disulfide and Cosan press 2:1 ratio copper removal can substantially reduce toxic thorn produced during the course of the reaction
Swash property gas, it is to avoid air is polluted, Environmental Safety coefficient is greatly improved；
2. being overcome using ferrous disulfide copper removal, Cosan is readily burned during copper removal, sulphur is converted into sulfur dioxide damage
The shortcoming lost, ferrous disulfide effective rate of utilization has obtained large increase, and the content to element sulphur in alloy and ferro element will not
Bring the influence of fluctuations of impurity content；
3. temperature rises to 420 ± 20 DEG C by 380 ± 20 DEG C during copper removal, it is to avoid the copper removal program for the cooling that adds water, effectively
Shorten production duration, reduce direct labor drags for slag operation intensity；
4. lead-antimony alloy remaining in pot can mix what is smelted as next batch with leaded discarded object after the completion of ingot casting
Raw material, effectively forms recycling for lead-antimony alloy.
In a word, the smelting process for the leaded discarded object configuration lead-antimony alloy that the present invention is provided has input cost low, safe
The advantage that environmentally friendly coefficient is high, production efficiency is high.
Brief description of the drawings
Fig. 1 is a kind of process chart of the smelting process of leaded discarded object configuration lead-antimony alloy of the present invention.
Embodiment
The present invention is further detailed explanation with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
By the leaded discarded object dress pots of 30t, once fill it up with, temperature control is completely melt at 325 DEG C to leaded discarded object；Again
360 DEG C are warming up to, 2.1kg rosin is added, mixer is put into and is stirred 15 minutes with 20Hz frequency, promote lead skim to be changed into black powder
Foam or fine particle shape, by mixer FREQUENCY CONTROL in 10Hz, the content for taking first sample to chemically examine copper with direct-reading spectrometer is
0.003%, drag for most scum silica frost；400 DEG C are continuously heating to, mixer FREQUENCY CONTROL is stirred in 35Hz, in whipping process, is pressed
(sulphur：Ferrous disulfide=2:1)：Copper=1:1 amount adds the mixture 0.9kg of Cosan and ferrous disulfide, stirs 15 minutes, treats
Scum silica frost becomes loose, not lumpd, darkly toner foam or fine particle shape, represents that reaction reaches terminal, by mixer FREQUENCY CONTROL
In 20Hz, it is respectively 0.0005% and 0.0025% to sample with the content of direct-reading spectrometer chemical examination copper and sulphur, drags for most scum silica frost；After
It is continuous to be warming up to 480 DEG C, 12kg sodium hydroxides are first added, 6kg sodium nitrate is added and carries out basic refining, stir 1.5 hours, sampling
It is respectively 1.75%, 0.01%, 0.005%, 0 with the content of direct-reading spectrometer chemical examination antimony, tin, arsenic, selenium, drags for most scum silica frost；After
It is continuous to be warming up to 500 DEG C, 360kg star antimonies are added, the FREQUENCY CONTROL of mixer is stirred 10 minutes in 15Hz, temperature control is existed
460 DEG C, 27kg pure tins are added, the FREQUENCY CONTROL of mixer is stirred 10 minutes in 15Hz, the pure arsenic of 28.5kg is first added, adds
3.6kg pure seleniums, the FREQUENCY CONTROL of mixer is stirred 10 minutes in 23Hz, and sampling chemically examines containing for each composition with direct-reading spectrometer
Amount is respectively antimony：2.95%th, tin：0.10%th, arsenic：0.1%th, selenium：0.012%th, copper：0.0008%th, bismuth：0.012%th, nickel：
0.0005%th, zinc：0.0005%th, iron：0.0005%th, sulphur：0.001%, lead is surplus, opens lead pump and starts ingot casting.
Embodiment 2：
By the leaded discarded object dress pots of 30t, once fill it up with, temperature control is completely melt at 327 DEG C to leaded discarded object；Again
380 DEG C are warming up to, 2.1kg rosin is added, mixer is put into and is stirred 20 minutes with 22Hz frequency, promote lead skim to be changed into black powder
Foam or fine particle shape, by mixer FREQUENCY CONTROL in 12Hz, the content for taking first sample to chemically examine copper with direct-reading spectrometer is
0.0032%, drag for most scum silica frost；420 DEG C are continuously heating to, mixer FREQUENCY CONTROL is stirred in 35Hz, in whipping process,
By (sulphur：Ferrous disulfide=2:1)：Copper=1:1 amount adds the mixture 0.96kg of Cosan and ferrous disulfide, stirs 20 minutes,
Treat that scum silica frost becomes loose, do not lumpd, darkly toner foam or fine particle shape, represent that reaction reaches terminal, unit frequency control will be stirred
System is in 20Hz, and it is respectively 0.0012% and 0.005% to sample with the content of direct-reading spectrometer chemical examination copper and sulphur, drags for most scum silica frost；
500 DEG C are continuously heating to, 12kg sodium hydroxides are first added, 6kg sodium nitrate is added and carries out basic refining, stir 1.8 hours, take
Sample is respectively 1.79%, 0.015%, 0.01%, 0 with the content of direct-reading spectrometer chemical examination antimony, tin, arsenic, selenium, drags for most scum silica frost；
520 DEG C are continuously heating to, 363kg star antimonies are added, the FREQUENCY CONTROL of mixer is stirred 12 minutes in 18Hz, temperature control is existed
480 DEG C, 31.5kg pure tins are added, the FREQUENCY CONTROL of mixer is stirred 12 minutes in 18Hz, the pure arsenic of 42kg is first added, adds
4.5kg pure seleniums, the FREQUENCY CONTROL of mixer is stirred 12 minutes in 25Hz, and sampling chemically examines containing for each composition with direct-reading spectrometer
Amount is respectively antimony：3%th, tin：0.12%th, arsenic：0.15%th, selenium：0.015%th, copper：0.001%th, bismuth：0.011%th, nickel：
0.0005%th, zinc：0.0005%th, iron：0.0005%th, sulphur：0.001%, lead is surplus, opens lead pump and starts ingot casting.
Embodiment 3：
By the leaded discarded object dress pots of 30t, once fill it up with, temperature control is completely melt at 330 DEG C to leaded discarded object；Again
400 DEG C are warming up to, 2.1kg rosin is added, mixer is put into and is stirred 30 minutes with 25Hz frequency, promote lead skim to be changed into black powder
Foam or fine particle shape, by mixer FREQUENCY CONTROL in 15Hz, the content for taking first sample to chemically examine copper with direct-reading spectrometer is
0.0035%, drag for most scum silica frost；440 DEG C are continuously heating to, mixer FREQUENCY CONTROL is stirred in 35Hz, in whipping process,
By (sulphur：Ferrous disulfide=2:1)：Copper=1:1 amount adds the mixture 1.05kg of Cosan and ferrous disulfide, stirs 30 minutes,
Treat that scum silica frost becomes loose, do not lumpd, darkly toner foam or fine particle shape, represent that reaction reaches terminal, unit frequency control will be stirred
System is in 20Hz, and it is respectively 0.0018% and 0.009% to sample with the content of direct-reading spectrometer chemical examination copper and sulphur, drags for most scum silica frost；
520 DEG C are continuously heating to, 12kg sodium hydroxides are first added, 6kg sodium nitrate is added and carries out basic refining, stir 2 hours, sampling
It is respectively 1.8%, 0.018%, 0.015%, 0 with the content of direct-reading spectrometer chemical examination antimony, tin, arsenic, selenium, drags for most scum silica frost；After
It is continuous to be warming up to 540 DEG C, 384kg star antimonies are added, the FREQUENCY CONTROL of mixer is stirred 15 minutes in 20Hz, temperature control is existed
480 DEG C, 32.1kg pure tins are added, the FREQUENCY CONTROL of mixer is stirred 15 minutes in 10Hz, the pure arsenic of 44.7kg are first added, then add
Enter 5.1kg pure seleniums, the FREQUENCY CONTROL of mixer is stirred 15 minutes in 27Hz, sampling chemically examines each composition with direct-reading spectrometer
Content is respectively antimony：3.08%th, tin：0.125%th, arsenic：0.164%th, selenium：0.017%th, copper：0.0015%th, bismuth：0.012%th,
Nickel：0.0005%th, zinc：0.0005%th, iron：0.0005%th, sulphur：0.001%, lead is surplus, opens lead pump and starts ingot casting.
Claims (8)
1. a kind of leaded discarded object configures the smelting process of lead-antimony alloy, it is characterised in that it includes following steps：
A, by leaded discarded object fill pot, once fill it up with, be capped pot cover, by temperature control 327 DEG C to leaded discarded objects completely melt
Change；
B, reduction slag making：380 ± 20 DEG C are continuously heating to, in terms of the weight of leaded discarded object, 0.007% rosin is added into pot
It is interior, it is put into mixer and is stirred 15-30 minutes with 20-25Hz frequency, promotes lead skim to be changed into black powder or fine particle shape, will
Mixer FREQUENCY CONTROL takes first sample to chemically examine the content of copper with direct-reading spectrometer, drags for most scum silica frost in 10-15Hz；
C, copper removal：420 ± 20 DEG C are continuously heating to, mixer FREQUENCY CONTROL is stirred in 35Hz, pressed（Sulphur：Ferrous disulfide=
2:1）：Copper=1:1 amount adds the mixture of ferrous disulfide and Cosan, stirs 15-30 minutes, treats that scum silica frost becomes loose, do not tied
Block, darkly toner foam or fine particle shape, represent that reaction reaches terminal, and by mixer FREQUENCY CONTROL in 20Hz, sampling is with straight
The content of spectrometer chemical examination copper and sulphur is read, most scum silica frost is dragged for；
D, stokehold refining：Be continuously heating to 500 ± 20 DEG C, in terms of the weight of leaded discarded object, by 0.04% sodium hydroxide and
0.02% sodium nitrate is added in pot, is stirred 1.5-2 hours, and sampling chemically examines antimony, tin, arsenic, the content of selenium with direct-reading spectrometer,
Drag for most scum silica frost；
E, alloy configuration：520 ± 20 DEG C are continuously heating to, with antimony in the content of antimony and lead-antimony alloy that are detected in step d
Star antimony addition that mathematic interpolation between component requirements content is drawn adds star antimony, by the FREQUENCY CONTROL of mixer 20Hz with
Interior stirring 10-15 minutes, by temperature control at 480 ± 20 DEG C, with tin in the content of tin and lead-antimony alloy that are detected in step d
Component requirements content between the pure tin addition that draws of mathematic interpolation add pure tin, by the FREQUENCY CONTROL of mixer in 20Hz
Within stir 10-15 minutes, with the component requirements content of arsenic, selenium in the arsenic detected in step d, the content of selenium and lead-antimony alloy
Between the pure arsenic that draws of mathematic interpolation, pure selenium addition add pure arsenic, pure selenium, the FREQUENCY CONTROL of mixer is stirred in 25Hz
10-15 minutes, the content of each composition was chemically examined in sampling with direct-reading spectrometer, is opened lead pump and is started ingot casting.
2. leaded discarded object according to claim 1 configures the smelting process of lead-antimony alloy, it is characterised in that：Described step
The content for the copper chemically examined in rapid b is not less than 0.003%.
3. leaded discarded object according to claim 1 configures the smelting process of lead-antimony alloy, it is characterised in that：Described step
The content for the copper chemically examined in rapid c is not more than 0.003%, and the content of sulphur is not more than 0.01%.
4. leaded discarded object according to claim 1 makes the smelting process of lead-antimony alloy, it is characterised in that：Described step
Sodium hydroxide is first added in rapid d, sodium nitrate is added.
5. leaded discarded object according to claim 1 configures the smelting process of lead-antimony alloy, it is characterised in that：Described step
Pure arsenic is first added in rapid e, pure selenium is added.
6. leaded discarded object according to claim 1 configures the smelting process of lead-antimony alloy, it is characterised in that：Described step
The content for the copper chemically examined in rapid b, which is not more than 0.003%, can directly carry out step d operation.
7. leaded discarded object according to claim 1 configures the smelting process of lead-antimony alloy, it is characterised in that：Described step
Repeat step c is needed not less than 0.003% for the content for the copper chemically examined in rapid c until the content of copper is not more than 0.003%.
8. leaded discarded object according to any one of claim 1 to 7 configures the smelting process of lead-antimony alloy, its feature exists
In：Lead-antimony alloy tailing remaining in pot after the completion of ingot casting can be with leaded discarded object mixing conduct in described step e
The raw material that next batch is smelted.
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| CN107619944A (en) * | 2016-07-16 | 2018-01-23 | 江西金洋金属有限公司 | A kind of method that impurity in lead is removed using decoppering agent |
| CN106282596B (en) * | 2016-08-27 | 2018-07-03 | 安徽省陶庄湖废弃物处置有限公司 | A kind of method that anaerobic pressurizing processes smelt lead bearing waste |
| CN106629633B (en) * | 2016-12-27 | 2019-05-17 | 郴州市金贵银业股份有限公司 | A method of dearsenification is refined from being precipitated in tellurium |
| CN110499428A (en) * | 2019-08-05 | 2019-11-26 | 襄阳金湛技术开发有限公司 | A kind of reviver decoppering agent and preparation method thereof |
| CN111751298B (en) * | 2020-07-21 | 2022-07-15 | 骆驼集团蓄电池研究院有限公司 | Method for measuring content of non-metal elements in crude lead |
| CN112095018B (en) * | 2020-08-11 | 2021-08-13 | 大连理工大学 | Method for controlling components in process of refining high-temperature alloy by electron beam |
| CN112391529A (en) * | 2020-10-15 | 2021-02-23 | 襄阳市立强机械有限公司 | Regenerated lead and regenerated antimonic acid alkali balance comprehensive smelting process |
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| CN101792873A (en) * | 2010-03-26 | 2010-08-04 | 如皋市天鹏冶金有限公司 | Low-stibium multicomponent lead alloy and production technology and applications thereof |
| CN102011015A (en) * | 2010-12-21 | 2011-04-13 | 株洲冶炼集团股份有限公司 | Method for removing arsenic, antimony and copper by refining raw lead |
| CN103667737A (en) * | 2013-12-31 | 2014-03-26 | 湖南省桂阳银星有色冶炼有限公司 | Primary pyro-refining method for lead bullions |
| CN104674018A (en) * | 2014-12-22 | 2015-06-03 | 芜湖市民泰铜业有限责任公司 | Method for chemical copper removal of wet lead |
| CN105087936A (en) * | 2015-04-09 | 2015-11-25 | 湖北金洋冶金股份有限公司 | Low-temperature detinning method for secondary lead bullion |
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