CN104611571B - A kind of converter nitre slag melting technique - Google Patents

A kind of converter nitre slag melting technique Download PDF

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Publication number
CN104611571B
CN104611571B CN201410849479.6A CN201410849479A CN104611571B CN 104611571 B CN104611571 B CN 104611571B CN 201410849479 A CN201410849479 A CN 201410849479A CN 104611571 B CN104611571 B CN 104611571B
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nitre
slag
melting
lead
stage
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CN104611571A (en
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许俊波
张伟萍
胡建平
娄可柏
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Zhejiang Tianneng Power Materials Co Ltd
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Zhejiang Tianneng Power Materials Co Ltd
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    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention discloses a kind of converter nitre slag melting technique, this technique includes: puts into iron filings and breeze in nitre slag, carries out melting after stirring in confined conditions；The initial temperature of described melting is 440～460 DEG C, and final temperature is 895～905 DEG C, and smelting time is 120～145min.The present invention carries out low temperature smelting to nitre slag in confined conditions, reduces environmental pollution；Using iron filings as catalyst, breeze is as reducing agent, and both of which simplicity is easy to get, with low cost, reduces smelting cost；Can directly reclaim the lead of about 90% in efficient recovery nitre slag after melting of the present invention, the lead of residue 6% is collected by flue, and other are collected by melting slag, and overall recovery is up to 98%；And reclaim the purity of lead also more than 99%.

Description

A kind of converter nitre slag melting technique
Technical field
The present invention relates to a kind of lead recovery process, be specifically related to a kind of converter nitre slag melting technique.
Background technology
As conduction electric current and the grid of support active substance, since lead-acid accumulator comes out, warp Many technical improvement are gone through.Initially, Plante is to use two blocks of stereotypes to make electrode, is placed in sulphuric acid Solution is electrolysed, makes the sense of current of electrolysis be continually changing, result make the capacitance of storage of stereotype by Cumulative add.1881, Sellon used Pb-Sb alloy to replace pure lead and makes electrode plate grid, makes battery The mechanical strength of pole plate dramatically increases, and this invention significantly improves the manufacturing process of lead battery, Become an important improvement in lead battery evolution.In the year more than 100 subsequently, people The performances such as the machinery of accumulator plate grid alloy, electrochemistry, burn into casting have been carried out a series of Improvement, have developed various series alloy to meet the use under varying environment.Currently used It is extensively lead-antimony alloy and lead-calcium alloy.
At present, the grid material that maintenance-free battery commonly uses most is lead-calcium alloy (Pb-Ca alloy), root According to calcium content can be divided into high calcium [w (Ca)=0.09%～0.13%], middle calcium [w (Ca)=0.06%～ 0.09%] and low calcium [w (Ca) ＜ 0.04%] alloy.Lead-calcium alloy is precipitation hardenable, i.e. exists Lead base matter is formed Pb3Ca, intermetallic precipitates becomes hardening network in lead base.Hardening net Network makes that (Pb-Ca alloy has good mechanical strength, slow down the dilatancy of grid.Pb-Ca The main advantage of alloy is exactly its overpotential of hydrogen evolution about high about 200mV than Pb-Sb alloy, thus When restrained effectively self discharge and the charging of battery, the hydrogen-separating quantity of negative pole, has preferable non-maintaining property Energy.The conductive capability of lead-calcium alloy is better than lead-antimony alloy, and its cryogenic property is aobvious is better than lead-antimony alloy.
In 20 years of past, Pb-Ca alloy is widely used in as in the accumulator of stand-by power supply, These batteries use in floating charge mode, infrequently discharge, crystallite dimension through corrosion to be stood, Use within the period of ten several years in accumulator, be resistant to grow up.
Lead-calcium alloy, in manufacturing process, needs interpolation to subtract the chemical composition slagging-off such as slag agent, can generate and contain The nitre slag that lead amount is higher.Prior art produces product man and typically directly discards nitre slag, seldom can be to nitre slag Carry out processing the lead wherein contained with recovery.But inherently there is certain risk in the transport of lead-containing material, Cost is high；And the existing processing method to nitre slag usually uses pyrometallurgical smelting, this smelting process Airborne dust is big, seriously polluted.Therefore, exploitation novel device or new technology carry out smelting to nitre slag is that gesture exists Must go.
Summary of the invention
The invention provides a kind of converter nitre slag melting technique, this smelting process efficiently solves lead pyrogenic process The problem of environmental pollution smelted.
A kind of converter nitre slag melting technique, including: in nitre slag, put into iron filings and breeze, stir After carry out melting in confined conditions；The initial temperature of described melting is 440～460 DEG C, final temperature Being 895～905 DEG C, smelting time is 90～115min.
The present invention carries out low temperature smelting to nitre slag in confined conditions, reduces environmental pollution；Use ferrum Bits are as catalyst, and breeze is as reducing agent, and both of which simplicity is easy to get, with low cost, reduces smelting It is smelt this.
As preferably, described melting included successively with the next stage:
(1) first stage: initial temperature is 440～460 DEG C, final temperature is 690～710 DEG C, molten The refining time is 25～30min；
(2) second stage: initial temperature is 690～710 DEG C, final temperature is 690～810 DEG C, molten The refining time is 13～17min；
(3) phase III: initial temperature is 690～810 DEG C, final temperature is 840～860 DEG C, molten The refining time is 13～17min；
(4) fourth stage: initial temperature is 840～860 DEG C, final temperature is 870～880 DEG C, molten The refining time is 13～17min；
In (5) the 5th stages: initial temperature is 870～880 DEG C, final temperature is 895～905 DEG C, molten The refining time is 13～17min；
(6) the 6th stages: melting 40～50min at 895～905 DEG C.
As further preferably, described melting included successively with the next stage:
(1) first stage: initial temperature is 450 DEG C, final temperature is 700 DEG C, and smelting time is 30min；
(2) second stage: initial temperature is 700 DEG C, final temperature is 800 DEG C, and smelting time is 15min；
(3) phase III: initial temperature is 800 DEG C, final temperature is 850 DEG C, and smelting time is 15min；
(4) fourth stage: initial temperature is 850 DEG C, final temperature is 875 DEG C, and smelting time is 15min；
In (5) the 5th stages: initial temperature is 875 DEG C, final temperature is 900 DEG C, and smelting time is 15min；
(6) the 6th stages: melting 45min at 900 DEG C.
In the present invention, described iron filings calculate according to formula (1) with the mass ratio of nitre slag:
X=a-0.005 × M1% (1)；
Wherein, X represents the mass ratio of iron filings and nitre slag, M1Represent the mass fraction of lead, a in nitre slag It is 0468～0.469.
As preferably, under 30～50 eye mesh screens, siftage ratio≤5% of described iron filings.
In the present invention, described breeze calculates according to formula (2) with the mass ratio of nitre slag:
Y=b-0.002 × M1% (2)；
Wherein, Y represents the mass ratio of breeze and nitre slag, M1Represent the mass fraction of lead, b in nitre slag It is 0.195～0.197.
As preferably, the particle diameter of described breeze is 3～5mm.Particle diameter is crossed conference and is caused smelting time to become Long.
As preferably, water content≤11% of described breeze.As further preferably, wet in summer etc. Spend higher under conditions of when carrying out melting, water content≤11% of described breeze；In the winter time etc. humidity is relatively When carrying out melting under conditions of low, water content≤8% of described breeze.
As preferably, fixed carbon content >=82% of described breeze.Fixed carbon is to participate in reduction in breeze The main active substances of reaction, keeps certain fixed carbon content, contributes to fully reclaiming lead.
After melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. reclaim lead； After reclaiming lead collection, collect upper strata slag.Compared with prior art, beneficial effects of the present invention For:
The present invention carries out low temperature smelting to nitre slag in confined conditions, reduces environmental pollution；Use ferrum Bits are as catalyst, and breeze is as reducing agent, and both of which simplicity is easy to get, with low cost, reduces smelting It is smelt this；The lead of about 90% in efficient recovery nitre slag, residue can be directly reclaimed after melting of the present invention The lead of 6% is collected by flue, and other are collected by melting slag, and overall recovery is up to 98%；And Reclaim the purity of lead also more than 99%.
Accompanying drawing explanation
Fig. 1 is the melting curves of embodiment 1；
Wherein, abscissa represents the time (min), and vertical coordinate represents temperature (DEG C).
Detailed description of the invention
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
In embodiments of the invention, nitre slag used siftage ratio under 40 eye mesh screens is all≤5%； The particle diameter of breeze used is 3～5mm, water content≤8%, fixed carbon content >=82%.And as do not made Specified otherwise, in embodiments of the invention, smelting temperature floats in ± 5 DEG C.
Embodiment 1
The present embodiment one converter nitre slag melting technique, including:
(1) 10 tons of nitre slags (lead tolerance is 78.25%) are taken, after stirring in advance with iron filings and breeze, Put in rotary furnace, under semi-enclosed condition, carry out melting；
The dosage M of iron filings is calculated according to formula (1)2It is 0.78 ton:
M 2 M 0 = 0.469 - 0.005 × M 1 % - - - ( 1 ) ;
The dosage M of breeze is calculated according to formula (2)3It is 0.4 ton:
M 3 M 0 = 0.196 - 0.002 × M 1 % - - - ( 2 ) ;
In formula (1) and (2), M0Represent nitre slag amount (being 1 ton in the present embodiment), M1 Represent the mass fraction (being 78.25 in the present embodiment) of lead in nitre slag.
Fusion process is as shown in table 1, Fig. 1:
The time in table 1 melting each stage and temperature
Stage Time Temperature
Feeding 0 450
First stage 30 700
Second stage 15 800
Phase III 15 850
Fourth stage 15 875
5th stage 15 900
6th stage 45 900
(2), after melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. return Receive lead；After reclaiming lead collection, collect upper strata slag.
Calculating the lead recovery (i.e. reclaiming the mass ratio of lead and nitre slag) of nitre slag, result of calculation is shown in Table 6； And detecting the component reclaiming lead, testing result is shown in Table 7.
Embodiment 2
The present embodiment one converter nitre slag melting technique, including:
(1) 10 tons of nitre slags (lead tolerance is 73.49%) are taken, after stirring in advance with iron filings and breeze, Put in rotary furnace, under semi-enclosed condition, carry out melting；
The dosage M of iron filings is calculated according to formula (1)2It is 1.01 tons:
M 2 M 0 = 0.468 - 0.005 × M 1 % - - - ( 1 ) ;
The dosage M of breeze is calculated according to formula (2)3It is 0.5 ton:
M 3 M 0 = 0.197 - 0.002 × M 1 % - - - ( 2 ) ;
In formula (1) and (2), M0Represent nitre slag amount (being 10 tons in the present embodiment), M1 Represent the mass fraction (being 73.49 in the present embodiment) of lead in nitre slag.Fusion process is as shown in table 2:
The time in table 2 melting each stage and temperature
Stage Time Temperature
Feeding 0 440
First stage 30 690
Second stage 15 790
Phase III 15 840
Fourth stage 15 870
5th stage 15 895
6th stage 45 895
(2), after melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. return Receive lead；After reclaiming lead collection, collect upper strata slag.
Calculating the lead recovery (i.e. reclaiming the mass ratio of lead and nitre slag) of nitre slag, result of calculation is shown in Table 6； And detecting the component reclaiming lead, testing result is shown in Table 7.
Embodiment 3
The present embodiment one converter nitre slag melting technique, including:
(1) 10 tons of nitre slags (lead tolerance is 76.62%) are taken, after stirring in advance with iron filings and breeze, Put in rotary furnace, under semi-enclosed condition, carry out melting；
The dosage M of iron filings is calculated according to formula (1)2It is 0.86 ton:
M 2 M 0 = 0.469 - 0.005 × M 1 % - - - ( 1 ) ;
The dosage M of breeze is calculated according to formula (2)3It is 0.42 ton:
M 3 M 0 = 0.195 - 0.002 × M 1 % - - - ( 2 ) ;
In formula (1) and (2), M0Represent nitre slag amount (being 10 tons in the present embodiment), M1 Represent the mass fraction (being 76.62 in the present embodiment) of lead in nitre slag.
Fusion process is as shown in table 3:
The time in table 3 melting each stage and temperature
Stage Time Temperature
Feeding 0 460
First stage 30 710
Second stage 15 810
Phase III 15 860
Fourth stage 15 880
5th stage 15 905
6th stage 45 905
(2), after melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. return Receive lead；After reclaiming lead collection, collect upper strata slag.
Calculating the lead recovery (i.e. reclaiming the mass ratio of lead and nitre slag) of nitre slag, result of calculation is shown in Table 6； And detecting the component reclaiming lead, testing result is shown in Table 7.
Embodiment 4
The present embodiment one converter nitre slag melting technique, including:
(1) 10 tons of nitre slags (lead tolerance is 76.35%) are taken, after stirring in advance with iron filings and breeze, Put in rotary furnace, under semi-enclosed condition, carry out melting；
The dosage M of iron filings is calculated according to formula (1)2It is 0.86 ton:
M 2 M 0 = 0.469 - 0.005 × M 1 % - - - ( 1 ) ;
The dosage M of breeze is calculated according to formula (2)3It is 0.43 ton:
M 3 M 0 = 0.196 - 0.002 × M 1 % - - - ( 2 ) ;
In formula (1) and (2), M0Represent nitre slag amount (being 10 tons in the present embodiment), M1 Represent the mass fraction (being 76.35 in the present embodiment) of lead in nitre slag.
Fusion process is as shown in table 4:
The time in table 4 melting each stage and temperature
Stage Time Temperature
Feeding 0 450
First stage 25 700
Second stage 13 800
Phase III 13 850
Fourth stage 13 875
5th stage 13 900
6th stage 43 900
(2), after melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. return Receive lead；After reclaiming lead collection, collect upper strata slag.
Calculating the lead recovery (i.e. reclaiming the mass ratio of lead and nitre slag) of nitre slag, result of calculation is shown in Table 6； And detecting the component reclaiming lead, testing result is shown in Table 7.
Embodiment 5
The present embodiment one converter nitre slag melting technique, including:
(1) take 1 ton of nitre slag (lead tolerance is 75.97%), put in rotary furnace, throw in nitre slag Enter iron filings and breeze, after stirring, carry out melting in confined conditions；
The dosage M of iron filings is calculated according to formula (1)2It is 0.089 ton:
M 2 M 0 = 0.469 - 0.005 × M 1 % - - - ( 1 ) ;
The dosage M of breeze is calculated according to formula (2)3It is 0.045 ton:
M 3 M 0 = 0.197 - 0.002 × M 1 % - - - ( 2 ) ;
In formula (1) and (2), M0Represent nitre slag amount (being 10 tons in the present embodiment), M1 Represent the mass fraction (being 75.97 in the present embodiment) of lead in nitre slag.
Fusion process is as shown in table 5:
The time in table 5 melting each stage and temperature
Stage Time Temperature
Feeding 0 450
First stage 30 700
Second stage 17 800
Phase III 17 850
Fourth stage 17 875
5th stage 17 900
6th stage 47 900
(2), after melting terminates, open and put lead mouth bottom rotary furnace, collect lower floor's melting thing and i.e. return Receive lead；After reclaiming lead collection, collect upper strata slag.
The lead direct recovery rate of calculating nitre slag: lead direct recovery rate=go out lead rate/leaded rate of raw material, calculates The results are shown in Table 6；And detecting the component reclaiming lead, testing result is shown in Table 7.
The lead direct recovery rate of each embodiment of table 6
Embodiment The leaded rate of raw material (%) Go out lead rate (%) Direct recovery rate (%)
Embodiment 1 78.25% 66.65% 85.18%
Embodiment 2 73.49% 66.95% 91.10%
Embodiment 3 76.62% 70.31% 91.76%
Embodiment 4 76.35% 68.61% 89.86%
Embodiment 5 75.97% 68.19% 89.76%
From table 6, after each embodiment melting, the lead recovery of nitre slag all reaches more than 85%, Close to 90%.
The each embodiment of table 7 reclaims the component testing result of lead
Component Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Pb 99.55077 99.52412 99.44919 99.24049 99.44434
Sn 0.19647 0.30199 0.40375 0.54004 0.32114
Cu 0.15503 0.02174 0.02007 0.12001 0.04572
Cd 0.00151 0.00227 0.0025 0.00727 0.00627
As 0.00597 0.00419 0.00074 0.00026 0.0017
Zn 0.00004 0.00056 0.00005 0.00007 0.00004
Ni 0.00373 0.00333 0.00041 0.00087 0.00293
Ag 0.00054 0.00036 0.00049 0.00065 0.00094
Sb 0.08454 0.14044 0.11354 0.07269 0.17203
Bi 0.00141 0.001 0.00117 0.00166 0.00201
From table 7, the purity reclaiming lead obtained through each embodiment melting all reaches more than 99%.

Claims (8)

1. a converter nitre slag melting technique, it is characterised in that including: put into iron filings in nitre slag And breeze, carry out melting after stirring in confined conditions；The initial temperature of described melting is 440～460 DEG C, final temperature is 895～905 DEG C, and smelting time is 90～115min；Described melting depends on Secondary include with the next stage:
(1) first stage: initial temperature is 440～460 DEG C, final temperature is 690～710 DEG C, molten The refining time is 25～30min；
(2) second stage: initial temperature is 690～710 DEG C, final temperature is 690～810 DEG C, molten The refining time is 13～17min；
(3) phase III: initial temperature is 690～810 DEG C, final temperature is 840～860 DEG C, molten The refining time is 13～17min；
(4) fourth stage: initial temperature is 840～860 DEG C, final temperature is 870～880 DEG C, molten The refining time is 13～17min；
In (5) the 5th stages: initial temperature is 870～880 DEG C, final temperature is 895～905 DEG C, molten The refining time is 13～17min；
(6) the 6th stages: melting 40～50min at 895～905 DEG C.
2. converter nitre slag melting technique as claimed in claim 1, it is characterised in that described melting Include successively with the next stage:
(1) first stage: initial temperature is 450 DEG C, final temperature is 700 DEG C, and smelting time is 30min；
(2) second stage: initial temperature is 700 DEG C, final temperature is 800 DEG C, and smelting time is 15min；
(3) phase III: initial temperature is 800 DEG C, final temperature is 850 DEG C, and smelting time is 15min；
(4) fourth stage: initial temperature is 850 DEG C, final temperature is 875 DEG C, and smelting time is 15min；
In (5) the 5th stages: initial temperature is 875 DEG C, final temperature is 900 DEG C, and smelting time is 15min；
(6) the 6th stages: melting 45min at 900 DEG C.
3. the converter nitre slag melting technique as described in as arbitrary in claim 1 or 2, it is characterised in that Described iron filings calculate according to formula (1) with the mass ratio of nitre slag:
X=a-0.005 × M1% (1)；
Wherein, X represents the mass ratio of iron filings and nitre slag, M1Represent the mass fraction of lead, a in nitre slag It is 0.468～0.469.
4. converter nitre slag melting technique as claimed in claim 3, it is characterised in that 30～50 Under eye mesh screen, siftage ratio≤5% of described iron filings.
5. the converter nitre slag melting technique as described in as arbitrary in claim 1 or 2, it is characterised in that Described breeze calculates according to formula (2) with the mass ratio of nitre slag:
Y=b-0.002 × M1% (2)；
Wherein, Y represents the mass ratio of breeze and nitre slag, M1Represent the mass fraction of lead, b in nitre slag It is 0.195～0.197.
6. converter nitre slag melting technique as claimed in claim 5, it is characterised in that described breeze Particle diameter be 3～5mm.
7. converter nitre slag melting technique as claimed in claim 5, it is characterised in that described breeze Water content≤11%.
8. converter nitre slag melting technique as claimed in claim 5, it is characterised in that described breeze Fixed carbon content >=82%.
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CN108300864B (en) * 2018-04-16 2019-10-15 天能集团（濮阳）再生资源有限公司 A kind of energy-saving hair lead refining process
CN115572836B (en) * 2022-09-19 2024-04-02 浙江天能电源材料有限公司 Smelting process of mixed high-carbon low-iron alkaline converter

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2309464A (en) * 1996-01-24 1997-07-30 Margulead Ltd Process for the manufacture of pure metallic lead from exhausted batteries.
CN102055045A (en) * 2010-12-10 2011-05-11 尚诚德 Energy-saving, environmental-protection and loss-reduction method for recovering and processing waste lead-acid storage battery
CN103937983A (en) * 2014-04-16 2014-07-23 湖北金洋冶金股份有限公司 Collaborative disposal method for leaded glass of waste cathode ray tubes and lead plaster of waste storage batteries

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2309464A (en) * 1996-01-24 1997-07-30 Margulead Ltd Process for the manufacture of pure metallic lead from exhausted batteries.
CN102055045A (en) * 2010-12-10 2011-05-11 尚诚德 Energy-saving, environmental-protection and loss-reduction method for recovering and processing waste lead-acid storage battery
CN103937983A (en) * 2014-04-16 2014-07-23 湖北金洋冶金股份有限公司 Collaborative disposal method for leaded glass of waste cathode ray tubes and lead plaster of waste storage batteries

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Denomination of invention: A converter nitrate slag smelting process

Effective date of registration: 20230905

Granted publication date: 20161207

Pledgee: Agricultural Bank of China Limited by Share Ltd. Changxing County branch

Pledgor: ZHEJIANG TIANNENG POWER SOURCE MATERIAL Co.,Ltd.

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