CN105970005B - A kind of high lead-antimony pyrogenic process antimony lead separation method - Google Patents
A kind of high lead-antimony pyrogenic process antimony lead separation method Download PDFInfo
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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
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- C22B30/02—Obtaining antimony
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Abstract
A kind of high lead-antimony pyrogenic process antimony lead separation method adds in covering adhesive in high lead-antimony, after heating melting, adds in deleading agent by several times, temperature control reaction, or stirring, antimony liquid pours out ingot casting,.The method of the present invention is widely used in high lead-antimony of the lead content 0.3~15.0%；The method of the present invention is good except lead effect, and except lead is efficient, when lead content is 10~15% in high lead-antimony, lead removal efficiency is up to 97.22%；As lead content ＜ 3% in high lead-antimony, lead content reaches the Sb99.70 standards in antimony slab GB/T1599 2014 down to 0.08% in antimony slab（Lead content ＜ 0.15%）；Covering adhesive used in the method for the present invention repeats utilization, environmentally protective；The deleading agent that the method for the present invention uses is at low cost；The method of the present invention technological process is short, easy to operate, and operating environment has obtained larger improvement, small investment, suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of stibium fire reduction refining methods, and in particular to a kind of high lead-antimony pyrogenic process antimony lead separation method.
Background technology
In antimony smelting process, high lead-antimony material of the lead tolerance 0.5~15.0% is often generated, such as using existing
Coarse antimony refining technology is lead slag-removed except lead generates, and the needle antimony of gained, leaded still 10.0% or so after synthetical recovery；In addition,
The antimony that jamesonite comes out through pyrometallurgical smelting is all the high needle antimony of lead tolerance.In antimony smelting industry, to how to handle this kind of height
Lead antimony has carried out long-term research of technique, and lead can be removed by failing to find always, while economically practicable technique again.
In the prior art, the method slowly waved and blown using low temperature carries out barium plumbate in high lead-antimony.Such as
CN1116232C discloses a kind of lead-antimony separation process, is that the antimony in high lead-antimony is strengthened oxygen abrupt oxidization into antimony oxide to come
It detaches lead and antimony, i.e., blows the method for cycle and realize the separation of lead antimony using waving to blow-oxidationreduction-and wave.But the method exists
The deficiencies of barium plumbate is not thorough, and time-consuming, and antimony volatilizing loss is big, high labor cost.
In addition, existing needle antimony is except lead technology is in deleading agent and except having certain limitation in lead effect.Such as
CN1455010A discloses a kind of fused-extracting refining lead-removing agent of antimony, and deleading agent composition is：Extractant Sb2O3Content 10~
60%、P2O5Content 20~60%, remaining is water, synergic reagent Sb2S3, along with fused salt.But there are 2 points for the technical solution
It is insufficient：（1）Deleading agent itself is expensive, Sb2O3、P2O5All it is expensive raw material；（2）Deleading agent is more suitable for low lead and contains
The needle antimony of amount in embodiment, handles the needle antimony that lead content is 4.10%.It is if higher thick with deleading agent processing lead content
Antimony, then cost is excessively high, and no economic benefit can be sayed.
CN1042653C disclose a kind of antimony except lead rifining method, the deleading agent which uses is molecular formula for SbnRm's
The silicon or boron of antimony or the oxysalt of phosphorus.But there are 2 points of deficiencies for the technical solution：（1）Deleading agent complex manufacturing technology, is removed
Lead agent is expensive；（2）Be not suitable for removing the lead in high lead-antimony, find out from embodiment, best except lead effect is, general
Lead tolerance is down to 0.18% by 2.4%, and to lead content, higher needle antimony can not then operate, and cost is excessively high.
CN102041399B discloses a kind of stibium fire refining deleading agent and application, and the composition of deleading agent is：Phosphorus contains
Oxygen acid 30~70% is measured, polyphosphoric acids sodium salt 20~60%, drier 2~10%, the sum of each component is 100%.But the technical side
There are 2 points of deficiencies for case：（1）Deleading agent is again without leaving hydrochlorate containing phosphorus oxygen, thus its is expensive；（2）It is also not suitable for removing
Remove the needle antimony that lead content is high, it is best except lead effect is in embodiment because of high lead-antimony except lead cost is excessively high, by lead tolerance by
2.3% is down to 0.32%.
CN1158906A discloses the method that antimonial lead removes lead with sulphur, the method be in antimonial lead addition element sulphur and
Sulfide obtains star metal and golden slag in metallurgical furnace melting, 600~800 DEG C of furnace temperature of control, wherein, deleading agent used is element sulphur
And sulfide（It is antimony trisulfide in example）, this two classes substance is all the substance of highly volatile at 600~800 DEG C.Therefore, should
There are following shortcomings for method：（1）Element sulphur and sulfide largely vapor away, dosage in addition to being used in addition to the part of lead
It is especially more；（2）The direct yield of antimony is relatively low, and direct yield minimum only 70.13% causes most antimony that cannot recycle, this damage
It loses, is unacceptable；（3）Since the fusing point of elementary sulfur is 112 DEG C, boiling point is 444.6 DEG C, and element sulphur is at 600~800 DEG C
Under, sulfur vapor easily with the oxygen combustion in air, not only except the effect of lead is very poor, but also generates sulfur dioxide toxic gas,
Cause environmental degradation.
Invention content
The technical problems to be solved by the invention are to overcome drawbacks described above of the existing technology, provide one kind and are suitable for
Barium plumbate in different lead content high lead-antimonies, it is good separating effect, efficient, at low cost, it is easy to operate, can industrialized production height
Lead stibium fire antimony lead separation method.
The technical solution adopted by the present invention to solve the technical problems is as follows：A kind of high lead-antimony pyrogenic process antimony lead separation method,
Covering adhesive is added in high lead-antimony, after heating melting, adds in deleading agent by several times, temperature control reaction, or stirring, antimony liquid pours out
Ingot casting,.
Further, the mass content of lead is 0.3~15.0% in the high lead-antimony.Lead in high lead-antimony is usually with simple substance
The form of lead exists, and therefore, by melting, lead is present in the form of simple substance in molten mass.
Further, the covering adhesive is sodium carbonate, sodium hydroxide, sodium sulphate, sodium chloride, calcium chloride or potassium chloride etc.
In two or more mixed things.Covering adhesive is also referred to as fused salt, and main function in the present invention has two, one is, by
More volatile in higher temperature reaction in antimony, inventor is the study found that utilize the proportion for covering adhesive and lead antimony molten mass
Difference（The proportion of fused salt is 2~3, and the proportion of molten mass is 6~7）, during the reaction, the covering adhesive of addition is reacting
It can be covered in high lead-antimony molten mass surface in the process, play the role of coverture, so as to effectively prevent the volatilization of molten metal antimony
And loss；The second is the vulcanized lead with generation bonds to form a kind of salt-mixture, floated since the salt-mixture proportion is lighter than melting antimony
On metallic antimony surface, therefore convenient for separation（Vulcanized lead proportion is 7.4~7.6, and metallic antimony proportion is 6.62）.However, except hydrogen-oxygen
Change other than sodium, the fusing point of above-mentioned single covering adhesive is all higher, and if the fusing point of sodium carbonate is 851 DEG C, sodium sulphate melts
Point is 884 DEG C, and the fusing point of sodium chloride is 801 DEG C, and the fusing point of calcium chloride is 782 DEG C, and the fusing point of potassium chloride is 770 DEG C.Inventor
If the study found that when covering adhesive more than above two is used cooperatively, the fusing point of mixture will reduce many,
Such as, sodium chloride is mixed with sodium carbonate, fusing point can be down to 650 DEG C or so, and three kinds or more of covering adhesive cooperation makes
With fusing point will reduce more.Since antimon point is 630.5 DEG C, high lead-antimony can be complete in the case of less than 700 DEG C
Portion forms molten condition, after the fusing point of covering adhesive reduces, can make even if at a lower temperature to react energy except lead
It is enough fully to carry out.
Further, the addition of the covering adhesive is the 10~20% of high lead-antimony material quality.If cover adhesive
Dosage is very few, then does not have the effect of coverture, causes the volatilization and loss of antimony, and cannot be whole by the vulcanized lead in molten mass
Bonding so that antimony lead separating effect is bad；If dosage crosses the waste at most causing covering adhesive.
Further, the deleading agent is ferrous disulfide and/or antimonous sulfide.Due to ferrous disulfide and antimonous sulfide
Thermal stability is not so good as vulcanized lead, therefore, the lead liquid in ferrous disulfide or antimonous sulfide and high lead-antimony molten condition（At this time molten
Lead in melt body exists with simple substance form）Easily reaction generation vulcanized lead, and can be stabilized.Specific chemical equation
It is as follows：
FeS2+Pb→FeS+PbS；
Sb2S3+3Pb→2Sb+3PbS。
The proportion of vulcanized lead is 7.4~7.6, compared with the proportion of metallic antimony（6.62）Greatly, vulcanized lead is mixed with fused salt by physics
Conjunction forms a kind of proportion scum silica frost also lighter than metallic antimony, the final separation realized with antimony liquid.Since fused salt is not sent out with vulcanized lead
Raw reaction, is only a kind of physical mixed, and fused salt is dissolved in water, and vulcanized lead is not soluble in water, therefore, the recyclable reuse of fused salt.
Except lead slag-removed after lead is made of vulcanized lead, a small amount of antimony trisulfide or ferrous sulfide, lead slag-removed after water logging returns blast furnace or roasting
Burn stove or open hearth recycling antimony and lead, the lead slag-removed easily processing obtained by the phosphoric acid deleading agent used compared with the prior art.
When antimonous sulfide does deleading agent, if without fused salt cover, antimonous sulfide suitable for remove lead reaction temperature
Under, element sulphur and antimony element are readily volatilized, and the volatilization of element sulphur reduces the efficiency except lead, have suitable fused salt to cover,
The efficiency except lead is not only increased, also avoids the loss of antimony；For ferrous disulfide, the covering of fused salt can also avoid sulfur vapor with
Oxygen combustion in air is conducive to enhancing except lead effect, and does not generate sulfur dioxide toxic gas（The proportion of antimonous sulfide
It is 4.64（Crystalline state）, ferrous disulfide proportion 4.5~4.8）.
Further, when the mass content of lead in high lead-antimony >=3.0%, the addition of the deleading agent removes lead matter to be theoretical
1.5~5.0 times of amount；As the mass content ＜ 3.0% of lead in high lead-antimony, the addition of the deleading agent removes lead matter to be theoretical
5.0~10.0 times of amount.It when lead content is 3.0~15.0%, is equivalent to and tentatively removes lead, the excessive multiple of dosage is relatively low；And
When lead content is 0.3~3.0%, belong to depth except lead, excessive multiple needs higher, can be only achieved except lead purpose, this is by gold
Belong to what the balance number of lead in the melt determined.
In the present invention, as the mass content ＜ 3.0% of lead in high lead-antimony, the restriction to above-mentioned deleading agent dosage is applicable
In raw material high lead-antimony, the high lead-antimony of the mass content of lead >=3.0% is equally applicable to through once except after lead, the mass content ＜ of lead
When 3.0%, that is to say, that, can be through secondary except lead is further reduced in antimony slab when the mass content >=3.0% of lead in high lead-antimony
Lead content, so that reaching ideal effect.
Further, by 3~6 additions of the deleading agent point.Since reaction slowly carries out, if primary add in, that
, it is impossible to the deleading agent reacted is participated at once it is possible that decomposing or aoxidizing and lose, and therefore, adding in by several times can be more effectively sharp
Use deleading agent.
Further, the temperature of the temperature control reaction is 700~800 DEG C.If reaction temperature is excessively high, the vulcanized lead heat of production is steady
It is qualitative variation and reaction of decomposing, that is, react to the left side carry out, be unfavorable for remove lead；If reaction temperature is too low, reaction speed mistake
Slowly, it takes longer for that reaction could be completed.
Further, when the mass content of lead in high lead-antimony >=3.0%, the time of temperature control reaction is 120~180min；When
In high lead-antimony during the mass content ＜ 3.0% of lead, the time of temperature control reaction is 60~120min.Under the reaction time, it can allow
Metallic lead can react abundant with deleading agent, achieve the purpose that except lead.
Further, the number of the stirring is 4~6 times, every time 5~10min.The stirring can be used manual or pneumatically stir
It mixes, to accelerate except the progress of lead reaction.
After the completion of temperature control reaction, after antimony liquid is heated to 900~950 DEG C, then ingot casting is poured out, obtain star metal.
The method of the present invention has the beneficial effect that：
（1）The method of the present invention is widely used in lead content barium plumbate in 0.3~15.0% high lead-antimony；
（2）The method of the present invention is good except lead effect, except lead is efficient, when lead content is 10~15% in high lead-antimony, and lead removing
Rate is up to 97.22%；As lead content ＜ 3% in high lead-antimony, lead content reaches antimony slab GB/T1599- down to 0.08% in antimony slab
Sb99.70 standards in 2014（Lead content ＜ 0.15%）；
（3）Covering adhesive used in the method for the present invention repeats utilization, lead slag-removed to have obtained good comprehensive profit
With, it greatly reduces and smelts solid slag pollution on the environment, it is environmentally protective；
（4）The cost of deleading agent ferrous disulfide that the method for the present invention uses is only the 10~20% of phosphoric acid deleading agent；And
Antimony in deleading agent antimonous sulfide can enter in antimony liquid, not cause damages, and antimony therein realizes increment, therefore, except lead into
This is low；
（5）The method of the present invention technological process is short, easy to operate, and operating environment has obtained larger improvement, and small investment is suitable for
Industrialized production.
Specific embodiment
With reference to embodiment, the invention will be further described.
Ferrous disulfide used in the embodiment of the present invention is industrial ore, and wherein the mass content of ferrous disulfide is 70%, institute
The purity of the antimonous sulfide used is 95%；Chemical reagent used in other, unless otherwise specified, passes through routine business
Approach obtains.
Embodiment 1
By gained high lead-antimony after the lead slag-removed synthetical recoveries of 400g（Wherein, antimony content 83.68%, lead content 15.0%）It is put into
In 500mL crucibles, then by 30g sodium chloride and 50g sodium carbonate mixings（Cover 20.0% that binder dosage is antimony raw material）, covering
In high lead-antimony surface, it is placed in Muffle furnace after heating melting, by 83.5g ferrous disulfides（Deleading agent dosage is the 1.68 of theoretical value
Times）Points of 6 times additions, 700 DEG C of temperature control react 180min, hand operated mixing 6 times, each 10min in reaction process, after reaction,
Antimony liquid is warming up to 900 DEG C, antimony liquid is poured into ingot casting ingot casting, antimony slag is stayed in crucible, obtains antimony slab 324.2g, antimony slag 198g.
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 95.94% in antimony slab, lead content 2.60%；Antimony content is 10.56% in antimony slag, and lead contains
Measure is 25.64%；The smelting direct yield of antimony is 92.92%, and the removal efficiency of lead is 85.95%.
Embodiment 2
By gained high lead-antimony after the lead slag-removed synthetical recoveries of 505.7g（Wherein, antimony content 88.62%, lead content 10.14%）It puts
Enter in 500mL crucibles, then by 26g sodium chloride and 50g calcium chloride mixings（Cover 15.0% that binder dosage is antimony raw material）, cover
High lead-antimony surface is placed on, is placed in Muffle furnace after heating melting, by 97.6g ferrous disulfides（Deleading agent dosage is theoretical value
2.29 again）Points of 6 times additions, 720 DEG C of temperature control react 160min, and hand operated mixing 5 times in reaction process, each 9min, reaction terminates
Afterwards, antimony liquid is warming up to 910 DEG C, antimony liquid is poured into ingot casting ingot casting, antimony slag is stayed in crucible, obtains antimony slab 406.8g, antimony slag
251g。
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 98.12% in antimony slab, lead content 0.35%；Antimony content is 16.89% in antimony slag, and lead contains
Measure is 19.46%；The smelting direct yield of antimony is 89.07%, and the removal efficiency of lead is 97.22%.
Embodiment 3
By gained high lead-antimony after the lead slag-removed synthetical recoveries of 400g（Wherein, antimony content 88.62%, lead content 10.14%）It is put into
In 500mL crucibles, then by 13.8g sodium chloride and 26.2g sodium sulphate mixings（Cover 10.0% that binder dosage is antimony raw material）,
High lead-antimony surface is covered in, is placed in Muffle furnace after heating melting, by 117.6g antimonous sulfides（Deleading agent dosage is theoretical value
5.0 times）Points of 6 times additions, 740 DEG C of temperature control react 120min, hand operated mixing 4 times, each 8min in reaction process, reaction knot
Antimony liquid is warming up to 920 DEG C by Shu Hou, antimony liquid is poured into ingot casting ingot casting, antimony slag is stayed in crucible, obtains antimony slab 403.5g（Wherein,
Contain the antimony shifted from antimonous sulfide）, antimony slag 215.9g.
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 97.81% in antimony slab, lead content 1.70%；Antimony content is 16.08% in antimony slag, and lead contains
Measure is 15.83%；The smelting direct yield of antimony is 88.74%, and the removal efficiency of lead is 86.52%.
Embodiment 4
By 356g stibium trioxide furnace bottom water high lead-antimonies（Wherein, antimony content 95.01%, lead content 2.96%）It is put into 500mL crucibles,
Again by 24.5g sodium chloride and 43.5g potassium chloride mixings（Cover 19.1% that binder dosage is antimony raw material）, it is covered in high lead-antimony
Surface is placed in Muffle furnace after heating melting, by 45.8g ferrous disulfides（Deleading agent dosage is 5.24 times of theoretical value）Divide 6 times
It adds in, 760 DEG C of temperature control, reaction 120min, hand operated mixing 5 times, each 7min in reaction process, after reaction, by antimony liquid liter
Temperature pours into ingot casting ingot casting to 930 DEG C, by antimony liquid, and antimony slag is stayed in crucible, obtains antimony slab 315g, antimony slag 138.7g.
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 96.56% in antimony slab, lead content 0.09%；Antimony content is 19.05% in antimony slag, and lead contains
Measure is 7.23%；The smelting direct yield of antimony is 89.93%, and the removal efficiency of lead is 97.40%.
Embodiment 5
By embodiment 1 except the high lead-antimony 300g after lead（Antimony content 95.94%, lead content 2.60%）It is put into 500mL crucibles,
Again by 20g sodium chloride, 20g calcium chloride and 20g potassium chloride mixings（Cover 20.0% that binder dosage is antimony raw material）, it is covered in
High lead-antimony surface is placed in Muffle furnace after heating melting, by 63.5g ferrous disulfides（Deleading agent dosage is 9.81 times of theoretical value）
Points of 6 times additions, 780 DEG C of temperature control react 90min, hand operated mixing 5 times, each 5min in reaction process, after reaction, by antimony
Liquid is warming up to 940 DEG C, and antimony liquid is poured into ingot casting ingot casting, and antimony slag is stayed in crucible, obtains antimony slab 273.5g, antimony slag 108.5g.
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 97.00% in antimony slab, lead content 0.15%；Antimony content is 22.58% in antimony slag, and lead contains
Measure is 6.78%；The smelting direct yield of antimony is 91.39%, and the removal efficiency of lead is 94.74%.
Embodiment 6
By embodiment 2 except the high lead-antimony 390g after lead（Antimony content 98.12%, lead content 0.35%）It is put into 500mL crucibles,
Again by 27.6g sodium chloride and 50.3g calcium chloride mixings（Cover 20.0% that binder dosage is antimony raw material）, it is covered in high lead-antimony
Surface is placed in Muffle furnace after heating melting, by 7.8g antimonous sulfides（Deleading agent dosage is 9.85 times of theoretical value）Divide 3 times
It adds in, 800 DEG C of temperature control, reaction 60min, after reaction, antimony liquid is heated up for hand operated mixing 5 times, each 6min in reaction process
To 950 DEG C, antimony liquid is poured into ingot casting ingot casting, antimony slag is stayed in crucible, obtains antimony slab 380.3g（Wherein, containing from trisulfides two
The antimony shifted in antimony）, antimony slag 56.4g.
Antimony in gained antimony slab and antimony slag is detected with volumetric method, and lead therein is examined with atomic absorption spectrophotometry
It surveys, testing result is as follows：Antimony content is 99.12% in antimony slab, lead content 0.08%；Antimony content is 17.47% in antimony slag, and lead contains
Measure is 1.82%；The smelting direct yield of antimony is 97.13%, and the removal efficiency of lead is 77.47%.
Claims (8)
1. a kind of high lead-antimony pyrogenic process antimony lead separation method, it is characterised in that：Covering adhesive, heating melting are added in high lead-antimony
Afterwards, add in deleading agent by several times, temperature control reaction, or stirring, antimony liquid pours out ingot casting,；The quality of lead contains in the high lead-antimony
Measure is 0.3~15.0%；The covering adhesive is in sodium carbonate, sodium hydroxide, sodium sulphate, sodium chloride, calcium chloride or potassium chloride
Two or more mixed things；The addition of the covering adhesive is the 10~20% of high lead-antimony material quality；The deleading agent
For ferrous disulfide；When the mass content >=3.0% of lead in high lead-antimony, the addition of the deleading agent is to be theoretical except lead quality
1.5~5.0 times；As the mass content ＜ 3.0% of lead in high lead-antimony, the addition of the deleading agent removes lead quality for theory
5.0~10.0 times.
2. high lead-antimony pyrogenic process antimony lead separation method according to claim 1, it is characterised in that：The deleading agent is divided 3~6 times
It adds in.
3. high lead-antimony pyrogenic process antimony lead separation method according to claim 1 or claim 2, it is characterised in that：The temperature of the temperature control reaction
Spend is 700~800 DEG C.
4. high lead-antimony pyrogenic process antimony lead separation method according to claim 1 or claim 2, it is characterised in that：When the matter of lead in high lead-antimony
When measuring content >=3.0%, the time of temperature control reaction is 120~180min；As the mass content ＜ 3.0% of lead in high lead-antimony, control
The time of temperature reaction is 60~120min.
5. high lead-antimony pyrogenic process antimony lead separation method according to claim 3, it is characterised in that：When the quality of lead in high lead-antimony contains
During amount >=3.0%, the time of temperature control reaction is 120~180min；As the mass content ＜ 3.0% of lead in high lead-antimony, temperature control is anti-
The time answered is 60~120min.
6. high lead-antimony pyrogenic process antimony lead separation method according to claim 1 or claim 2, it is characterised in that：The number of the stirring is 4
~6 times, 5~10min every time.
7. high lead-antimony pyrogenic process antimony lead separation method according to claim 3, it is characterised in that：The number of the stirring is 4~6
It is secondary, 5~10min every time.
8. high lead-antimony pyrogenic process antimony lead separation method according to claim 4, it is characterised in that：The number of the stirring is 4~6
It is secondary, 5~10min every time.
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| CN109097589A (en) * | 2018-11-01 | 2018-12-28 | 锡矿山闪星锑业有限责任公司 | A method of lead is removed containing lead and tin metallurgy |
| CN109306410B (en) * | 2018-11-13 | 2021-03-02 | 锡矿山闪星锑业有限责任公司 | Method for separating antimony and lead from lead-containing antimony slag by pyrogenic process |
| CN111118306B (en) * | 2020-01-16 | 2021-09-17 | 昆明理工大学 | Method for removing sodium and sulfur from crude antimony and enriching gold |
| CN111679031A (en) * | 2020-04-28 | 2020-09-18 | 西北矿冶研究院 | Method for measuring antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method |
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