CN102417991B - Copper ashes melt oxidation chlorination-reduction reclaims copper and the method for obtained qualified molten iron - Google Patents
Copper ashes melt oxidation chlorination-reduction reclaims copper and the method for obtained qualified molten iron Download PDFInfo
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- CN102417991B CN102417991B CN201110380257.0A CN201110380257A CN102417991B CN 102417991 B CN102417991 B CN 102417991B CN 201110380257 A CN201110380257 A CN 201110380257A CN 102417991 B CN102417991 B CN 102417991B
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- copper
- copper ashes
- molten iron
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a kind of copper ashes melt oxidation chlorination-reduction and reclaim copper and the method for obtained qualified molten iron, by being come out of the stove by high temperature, copper ashes heats up, and add chlorizating agent, additive, after the abundant melting of copper ashes, pass into oxidizing gas wherein again, carry out the process of oxidation chlorination desulfurization decopper(ing), obtain melt liquid; The high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling; Under inert gas atmosphere, pass into fine coal, make fine coal under stirring of inert gas effect, mix with slag and fusion reduction reaction occurs, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature.Present method efficiently solves Sulfur Content in Hot Iron in the direct ironmaking technique of fusion and reduction of current copper ashes, shortcoming that copper content is higher, and achieves the high efficiente callback of copper resource in copper ashes, has good industrial prospect.
Description
Technical field
The present invention relates to a kind of hot copper ashes melt oxidation chlorination-reduction and reclaim copper and the method for obtained qualified molten iron, belong to resource and environment field.
Background technology
China's steel industry tempo is very fast in recent years, and its with a very important position in world's steel industry, Iron and Steel Production total amount occupies first place, the world always during the last ten years.But, China's iron ore resource situation can not meet the demand of steel industry far away, and domestic iron ore resource distribution has the defect that lean ore is many, the complex ore of multielement symbiosis is more and iron ore resource lacks, grade is low, another additional national steel enterprise production capacity is huge, iron ore demand rises year by year, import is interdependent, under the economic setting that iron ore price skyrockets, cause China's ironmaking cost to increase severely, weaken the profit margin of steel industry, had a strong impact on the development of China Steel industry.
Therefore, the supplemental resources finding a kind of iron ore be can yet be regarded as iron-smelting raw material and is solved an effective settling mode of China iron deposit stone resource long-term shortage.
According to statistics, produce the copper ashes that one ton of copper produces 2.2 tons, the copper output of China in 2007 is 3,500,000 tons, the amount of corresponding output copper ashes 7,700,000 tons, and the copper output of China in 2008 is about 3,710,000 tons, and the amount of output copper ashes is 8,160,000 tons as calculated.Iron content about 40% in copper ashes, calculates and knows that in copper ashes, iron has higher reclamation value.
In metallurgy of copper slag, chalybeate is mainly 2FeOSiO mutually
2(fayalite) and Fe
3o
4(magnetite), reclaim iron method in current copper ashes and mainly contain three kinds:
The first, oxide treatment is carried out in the molten state, by 2FeOSiO in copper ashes after copper ashes cooling
2(fayalite) changes Fe into
3o
4(magnetite), carries out cooling crushing-magnetic selection to copper ashes after process thereafter, Fe-riched phase and its recrement is separated, makes iron enrichment.Related documents proves, iron in copper ashes is reclaimed by this method, the enrichment of iron in magnetite in slag can be made to reach more than 85%, but there is following shortcoming in this kind of method: one is that oxidizing reaction later stage magnetite is separated out mutually in a large number, slag viscosity and fusing point raise, hinder reaction to proceed and magnetite phase agglomeration, cause iron yield lower; Two is that in copper ashes, iron resources, after magnetic concentration, is re-used as iron-smelting raw material and reduces, and treatment scheme is complicated; Three is high-temperature fusion oxide treatment again after being cooled by copper ashes, causes the waste of heat in process.The tapping temperature of copper ashes is 1150 ~ 1250 DEG C, and the specific heat capacity of copper ashes is approximately 1.1kJkg
-1k
-1, as calculated by copper ashes by tapping temperature cool to room temperature 25 DEG C time, the heat of China's copper smelting plant 2008 loss is approximately: 1.1 × 10
13~ 1.2 × 10
13kJ, carries out economy by thermal value and accounts, the calorific value according to mark coal: 29271.2kJkg
-1calculate, in conjunction with the price marking coal at present, the financial loss that annual China causes because of the calorific loss of copper ashes is at least 2.1 hundred million Renminbi, and it is extended to world wide, and its financial loss is more huge;
The second, Staged grinding and staged separation technique is adopted, there is the low shortcoming of iron recovery in slag (being less than 60%) in this method, reason be slag chalybeate mutually in magnetic oxygenated iron level less, only 20 ~ 30%, main chalybeate phase ferrosilicate enters mine tailing in magnetic separation process;
Three, melting reduction method is utilized, by 2FeOSiO in copper ashes
2(fayalite) and Fe
3o
4direct melting and reducing is metallic iron, and realizes slag sluicing system in the molten state.But there is the shortcoming of gained molten iron copper after copper ashes melting and reducing, sulphur content higher (sulphur average content higher than 0.6%, copper average content higher than 1%) in this technique.
Summary of the invention
The present invention is on copper ashes method for melting reduction iron making basis, make full use of sulphur and there is feature in copper ashes, solve and directly utilize the shortcoming that copper ashes ironmaking technique of fusion and reduction gained molten steel sulfur content is high, provide a kind of copper ashes melt oxidation chlorination-reduction to reclaim copper and the method for obtained qualified molten iron.
The present invention is realized by following technical proposal: a kind of copper ashes melt oxidation chlorination-reduction reclaims copper and the method for obtained qualified molten iron, through following each step:
(1) copper ashes of being come out of the stove by high temperature is warming up to 1500 ~ 1600 DEG C to reduce viscosity coefficient of dross, and be Lvization Ji ︰ copper ashes=1 ︰ 4 ~ 20 in mass ratio, mix with chlorizating agent, again in mass ratio for Tian Jia Ji ︰ copper ashes=1 ︰ 4 ~ 10 adds melting 40 ~ 60min after additive, after the abundant melting of copper ashes, pass into oxidizing gas 30 ~ 90min wherein with pressure 0.5 ~ 1.5MPa, carry out the process of oxidation chlorination desulfurization decopper(ing), obtain melt liquid; The high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling;
(2) under inert gas atmosphere, in step (1) gained melt liquid, pass into fine coal with pressure 0.3 ~ 1.0MPa, make fine coal under stirring of inert gas effect, mix with slag and fusion reduction reaction occurs, treat that fine coal intake is with mass ratio C/Fe
x+stop when (x=2,3) are 1.4 ~ 1.9 ︰ 1 passing into, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature.
The chlorizating agent of described step (1) is CaCl
2, NaCl, BaCl
2and/or AlCl
3.
The additive of described step (1) is CaF
2and/or BaF
2.
For reducing the chloridizing volatilization of chalybeate phase in described step (1), add CaO for CaO ︰ copper ashes=0.35 ~ 0.42 ︰ 1 in mass ratio more after the addition of the additives.
The oxidizing gas of described step (1) is air, oxygen-rich air or oxygen.
The rare gas element of described step (2) is nitrogen or argon gas.
The pulverized coal particle size of described step (2) is 40 ~ 60 orders.
The washing of described step (2) is contained obnoxious flavour in removing flue gas, as sulfurous gas, oxynitride.
The high-temperature flue gas formed during described step (2) melting and reducing through secondary combustion, waste heat recovery, dust removal process and washing, then enters air.
Through above steps, it is comparatively obvious that molten iron sulphur, copper content reduce effect.Desulfurization decopper(ing) completes in step (1), and the reaction occurred in process is:
xFeS+(x+1/2)O
2=Fe
xO+xSO
2(1)
CuS+O
2=CuO+SO
2(2)
Cu
2S+O
2=Cu
2O+SO
2(3)
CaCl
2+1/2O
2+xSiO
2=CaO·xSiO
2+Cl
2(4)
Cl
2+Cu
2S=2CuCl+1/2S
2(5)
Cl
2+Cu
2O=2CuCl+1/2O
2(6)
After chlorination desulfurization decopper(ing) to be oxidized has reacted, under an inert atmosphere, fine coal is sprayed into in slag, Fe containing component generation fusion reduction reaction in slag, reacts and be:
[C]+Fe
3O
4=3(FeO)+CO（7）
[C]+Fe
2O
3=2(FeO)+CO（8）
[C]+(FeO)=[Fe]+CO（9）
CO+(FeO)=[Fe]+CO
2（10）
CO
2+[C]=2CO（11）
The high-temperature flue gas produced is overflowed from slag blanket, causes the disturbance in molten bath; The violent disturbance in molten bath increases contacting of high-temperature area above molten slag layer and reductive agent (coal dust) and molten slag layer, enhances molten copper slag reduction kinetics condition.The molten iron generated is deposited to rapidly bottom molten bath higher than slag due to himself proportion, thick high-temperature slag covers the top of iron bath, thus make the molten iron restored avoid again oxidized possibility, also insulation effect is served to molten bath simultaneously, achieve slag sluicing system.Along with constantly carrying out of reaction, interval improves the position that stirring of inert gas is robbed, and makes it to reach best to the stirring in molten bath.After having reacted, will the high temperature liquid iron that be smelted and slag is released by iron notch and slag notch respectively.
The present invention makes full use of high temperature and to come out of the stove the feature that sulphur thing in the high temperature sensible heat of copper ashes and slag mutually oxidizablely removes, copper thing is easy to chloridizing volatilization mutually, utilize hot copper ashes melt oxidation chlorination-reduction to reclaim copper and obtained qualified molten iron, the beneficial effect that the present invention possesses and advantage are:
(1) adopt melt oxidation method to carry out copper ashes desulfurization, because reaction is carried out under liquid environment in process, its dynamic conditions is better, and copper ashes desulphurization reaction carries out comparatively thorough;
(2) high temperature copper ashes directly carries out melting and reducing, and heat loss is less, efficiently utilizes the high temperature sensible heat of copper ashes of coming out of the stove;
(3) efficiently solve Sulfur Content in Hot Iron in the direct ironmaking technique of fusion and reduction of current copper ashes, shortcoming that copper content is higher, and achieve the high efficiente callback of copper resource in copper ashes, have good industrial prospect.
Embodiment
Illustrate content of the present invention further below in conjunction with embodiment, but these examples do not limit the scope of the invention.
Embodiment 1
(1) high temperature to be come out of the stove copper ashes (component: FeO=48.5%, Fe
3o
4=5.7%, CaO=2.83%, SiO
2=28.62%, S=0.51%) be warming up to 1600 DEG C to reduce viscosity coefficient of dross, and be Lvization Ji ︰ copper ashes=1 ︰ 4 in mass ratio, with chlorizating agent CaCl
2mix, then add CaF for Tian Jia Ji ︰ copper ashes=1 ︰ 10 in mass ratio
2rear melting 40min, for reducing the chloridizing volatilization of chalybeate phase, then adds CaO for CaO ︰ copper ashes=0.35 ︰ 1 in mass ratio, after the abundant melting of copper ashes, pass into oxygen 50min wherein with pressure 1MPa, carry out the process of oxidation chlorination desulfurization decopper(ing), obtain melt liquid; The high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling;
(2) under a nitrogen, in step (1) gained melt liquid, passing into granularity with pressure 0.3MPa is 40 object fine coal, makes fine coal under nitrogen gas stirring effect, mixes reduction reaction occurs with slag, treats that fine coal intake is with mass ratio C/Fe
x+stop when (x=2,3) are 1.6 ︰ 1 passing into, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature and slag; The high-temperature flue gas that period is formed is through secondary combustion, waste heat recovery, dust removal process and washing, and in removing flue gas, contained obnoxious flavour, as sulfurous gas, oxynitride, then enters air.
Molten iron S content is 0.028% by analysis, and under the prerequisite utilizing copper ashes ironmaking technique of fusion and reduction significantly to reduce in molten bath basicity than before, sulphur content also significantly reduces.
Embodiment 2
(1) high temperature to be come out of the stove copper ashes (component: FeO=48.3%, Fe
3o
4=5.9%, CaO=2.77%, SiO
2=28.54%, S=0.50%) be warming up to 1550 DEG C to reduce viscosity coefficient of dross, and be Lvization Ji ︰ copper ashes=1 ︰ 10 in mass ratio, with NaCl and BaCl
2mix, then add BaF for Tian Jia Ji ︰ copper ashes=1 ︰ 8 in mass ratio
2rear melting 55min, for reducing the chloridizing volatilization of chalybeate phase, then adds CaO for CaO ︰ copper ashes=0.42 ︰ 1 in mass ratio, after the abundant melting of copper ashes, pass into air 90min wherein with pressure 0.5MPa, carry out the process of oxidation chlorination desulfurization decopper(ing), obtain melt liquid; The high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling;
(2) under argon gas, in step (1) gained melt liquid, passing into granularity with pressure 0.8MPa is 50 object fine coal, makes fine coal under argon gas stirring action, mixes reduction reaction occurs with slag, treats that fine coal intake is with mass ratio C/Fe
x+stop when (x=2,3) are 1.4 ︰ 1 passing into, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature and slag; The high-temperature flue gas that period is formed is through secondary combustion, waste heat recovery, dust removal process and washing, and in removing flue gas, contained obnoxious flavour, as sulfurous gas, oxynitride, then enters air.
Molten iron S content is 0.037% by analysis, and under the prerequisite utilizing copper ashes ironmaking technique of fusion and reduction significantly to reduce in molten bath basicity than before, sulphur content also significantly reduces.
Embodiment 3
(1) copper ashes of being come out of the stove by high temperature is warming up to 1500 DEG C to reduce viscosity coefficient of dross, and is Lvization Ji ︰ copper ashes=1 ︰ 20 in mass ratio, with AlCl
3mix, then add addition of C aF for Tian Jia Ji ︰ copper ashes=1 ︰ 4 in mass ratio
2and BaF
2rear melting 60min, after the abundant melting of copper ashes, passes into oxygen-rich air 30min wherein with pressure 1.5MPa, carries out the process of oxidation chlorination desulfurization decopper(ing), obtains melt liquid; The high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling;
(2) under a nitrogen, in step (1) gained melt liquid, passing into granularity with pressure 1.0MPa is 60 object fine coal, makes fine coal under nitrogen gas stirring effect, mixes reduction reaction occurs with slag, treats that fine coal intake is with mass ratio C/Fe
x+stop when (x=2,3) are 1.9 ︰ 1 passing into, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature and slag; The high-temperature flue gas that period is formed is through secondary combustion, waste heat recovery, dust removal process and washing, and in removing flue gas, contained obnoxious flavour, as sulfurous gas, oxynitride, then enters air.
Molten iron S content is 0.027% by analysis, and under the prerequisite utilizing copper ashes ironmaking technique of fusion and reduction significantly to reduce in molten bath basicity than before, sulphur content also significantly reduces.
Claims (8)
1. copper ashes melt oxidation chlorination-reduction reclaims copper and a method for obtained qualified molten iron, it is characterized in that through following each step:
(1) copper ashes of being come out of the stove by high temperature is warming up to 1500 ~ 1600 DEG C, and be Lvization Ji ︰ copper ashes=1 ︰ 4 ~ 20 in mass ratio, mix with chlorizating agent, more in mass ratio for Tian Jia Ji ︰ copper ashes=1 ︰ 4 ~ 10 adds melting 40 ~ 60min after additive, described additive is CaF
2and/or BaF
2; After the abundant melting of copper ashes, pass into oxidizing gas 30 ~ 90min wherein with pressure 0.5 ~ 1.5MPa, the high-temperature flue gas that period is formed is by the copper in recovered flue gas after gradient cooling; Described high temperature is come out of the stove the metallurgy of copper slag produced when copper ashes is production of copper, and in this metallurgy of copper slag, chalybeate is mainly 2FeOSiO mutually
2and Fe
3o
4;
(2) under inert gas atmosphere, in step (1) gained melt liquid, pass into fine coal with pressure 0.3 ~ 1.0MPa, treat that fine coal intake is with mass ratio C/Fe
x+stop when (x=2,3) are 1.4 ~ 1.9 ︰ 1 passing into, leave standstill after slag is separated with molten iron, obtain the qualified molten iron of high temperature.
2. method according to claim 1, is characterized in that: the chlorizating agent of described step (1) is CaCl
2, NaCl, BaCl
2and/or AlCl
3.
3. method according to claim 1, is characterized in that: described step adds CaO for CaO ︰ copper ashes=0.35 ~ 0.42 ︰ 1 in (1) after the addition of the additives more in mass ratio.
4. method according to claim 1, is characterized in that: the oxidizing gas of described step (1) is air, oxygen-rich air or oxygen.
5. method according to claim 1, is characterized in that: the rare gas element of described step (2) is nitrogen or argon gas.
6. method according to claim 1, is characterized in that: the pulverized coal particle size of described step (2) is 40 ~ 60 orders.
7. method according to claim 1, is characterized in that: the high-temperature flue gas formed during described step (2) melting and reducing through secondary combustion, waste heat recovery, dust removal process and washing, then enters air.
8. method according to claim 7, is characterized in that: the washing of described step (2) is contained obnoxious flavour in removing flue gas.
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| CN201110380257.0A CN102417991B (en) | 2011-11-25 | 2011-11-25 | Copper ashes melt oxidation chlorination-reduction reclaims copper and the method for obtained qualified molten iron |
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| CN102417991B true CN102417991B (en) | 2016-02-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952952B (en) * | 2012-09-26 | 2014-08-20 | 东北大学 | Method for directly restoring and recovering copper iron from smelting copper slag |
| CN103276222A (en) * | 2013-05-15 | 2013-09-04 | 大冶有色金属有限责任公司 | Technical method and device for treating diaphragm and freezing layer in subsiding electric furnace through pulverized coal in copper pyrometallurgical process |
| CN103572069B (en) * | 2013-11-18 | 2015-06-03 | 海安县鹰球粉末冶金有限公司 | Batching and smelting method for smelting blister copper by scrap copper |
| CN107475476A (en) * | 2017-06-28 | 2017-12-15 | 昆明理工大学 | A kind of method that copper-containing residue chlorination melting and reducing one-step method prepares the pig iron |
| CN111394593B (en) * | 2020-05-08 | 2021-04-23 | 中南大学 | Method for reducing fluorine and chlorine content in copper smelting flue gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555551A (en) * | 2009-05-22 | 2009-10-14 | 昆明理工大学 | Method for comprehensively recovering Fe, Cu and Si from copper smelting slag |
| CN101824505A (en) * | 2010-05-10 | 2010-09-08 | 昆明理工大学 | Method for producing low-sulfur molten iron in one step by smelting and reducing copper slag |
| CN101886154A (en) * | 2010-07-02 | 2010-11-17 | 昆明理工大学 | Method for preparing low-copper molten iron by mixed melting reduction of copper slag and iron ore |
-
2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555551A (en) * | 2009-05-22 | 2009-10-14 | 昆明理工大学 | Method for comprehensively recovering Fe, Cu and Si from copper smelting slag |
| CN101824505A (en) * | 2010-05-10 | 2010-09-08 | 昆明理工大学 | Method for producing low-sulfur molten iron in one step by smelting and reducing copper slag |
| CN101886154A (en) * | 2010-07-02 | 2010-11-17 | 昆明理工大学 | Method for preparing low-copper molten iron by mixed melting reduction of copper slag and iron ore |
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