CN101144135B - Technique for producing environment-friendly nickel/cobalt/iron alloy and system thereof - Google Patents
Technique for producing environment-friendly nickel/cobalt/iron alloy and system thereof Download PDFInfo
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Abstract
The present invention relates to an environment friendly nickel/cobalt/iron alloy production process and a system. The process comprises the following steps: in a smelting furnace, under the conditionof charging oxygen containing gas, raw material containing ferro phosphorus is mixed and smelted with material containing waste nickel and waste cobalt to get mixed meltwater, thereby phosphorus in the raw material is burned for heat supply, and iron in the raw material is used as reductant to reduce nickel cobalt in the oxidation state to be the nickel cobalt in the simple substance state or thelow valence state; slaging medium is added into the mixed meltwater, to create nickel cobalt iron meltwater with slag and nickel cobalt iron as the main components, the slag has small specific gravity, and the nickel cobalt iron has large specific gravity; the slag is discharged from the middle part of the smelting furnace, and the create nickel cobalt iron meltwater is led out of the lower partof the smelting furnace, to get the nickel/cobalt/iron alloy after quick chilling. The production process and the system of the present invention use waste nickel and waste cobalt as raw materials, and adopt an energy saving, consumption reducing and environment friendly method to produce the nickel/cobalt/iron alloy, the product can replace a pure nickel plate and a cobalt sheet, and the presentinvention provides the nickel/cobalt/iron intermediate alloy with low cost for the alloy industries of stainless steel, etc.
Description
Technical field
The present invention relates to a kind of metallurgical production technology and equipment, more particularly, the present invention relates to a kind of recovery production technology and equipment of nickeliferous and/or cobalt raw material or waste material.
Background technology
Nickel has the physico-chemical property of many excellences, thereby is applied on many fields and the product: the main component that for example becomes many magneticsubstances because of its good magnetic; Nickel also has good oxidation-resistance, and in air, nickel surface forms the NiO film, can stop further oxidation.Experimental results show that: purity is 99% nickel, in 20 years iron mold can not take place, the resistance to corrosion of nickel is very strong, especially the resistance to corrosion to caustic alkali is strong, the corrosion speed in nickel every year is no more than 25 microns in 50% boiling soda lye, thereby nickel is used for making various types of stainless steels, non-retentive alloy and structural alloy steel in a large number, and elements such as nickel and chromium, copper, aluminium, cobalt can be formed refractory alloy, electrical alloy and non-corrosive metal etc.Nichrome is (as Ni-Cr
2O) high thermotolerance and big resistance are arranged,, can be used as the electrical heating element of electric furnace, electric iron, electric iron etc. with the pyroelectrics (resistance wire) that it is done, can be 1100 ℃ of following long term operations; The intensity of nickel and plasticity are also fine, can bear various press working.In addition, nickel is also more and more to be used for field of chemical power source, for example in nickel-cadmium, nickel-hydrogen cell, the lithium ion battery; Porous nickel sheet still is a kind of catalyst of having many uses.This shows, also increasing as the demand of the metallic nickel of various products materials.
Especially in recent years, along with the widespread use of stainless steel at civil area, global stainless steel becomes the biggest market of nickel, and usage quantity accounts for more than 50% of dimensions of market of nickel more than 300,000 tons, causes the global anxiety of nickel resources, and the nickel valency continues to rise suddenly and sharply.Traditional stainless steel art is to add pure nickel plate, cobalt sheet in iron, carries out high melt, rolling processing forms, and therefore, along with rising suddenly and sharply of, nickel resources price, it is difficult to cause stainless steel manufacturing concern to manage.The nickel raw material of developing low-cost becomes one of outlet of stainless steel industry.
And the production of nickel in the prior art, mainly the ore with nickel is a raw material, by electrolytic process production: normally make thick nickel anode as raw material with nickeliferous electrolytic nickel slag or pyrite cinder etc., obtain electrolytic nickel through dissolving, purification and anode electrolysis method at negative electrode, perhaps make nickelous chloride, nickel sulfate solution with above-mentioned raw materials, through the insoluble anode electrolytic process, make electrodeposition of nickel on negative electrode, obtain electrolytic nickel; Then electrolytic nickel is scraped from negative electrode and form the nickel sheet.Electrolysis legal system nickel sheet can obtain the very high nickel sheet of purity, and still, the energy consumption of electrolysis legal system nickel technology is very high, and in electrolytic process, vitriol, the hydrochloride of nickel volatilize acid mist, all can produce quite serious pollution to production environment and living environment.So country restriction: in densely populated, the regional technology that does not allow investment construction electrolysis legal system nickel of energy scarcity so that now can only be in Gansu, the industrial equipments of scarcely populated, economically underdeveloped area's investment construction electrolytic nickel sheet such as Sichuan, Xinjiang.So just greatly limit the development of this industry, and caused the seriously in short supply of nickel tablet raw material supply.Simultaneously, be that the master produces the nickel raw material with the ore, cause the transition consumption of former ore resources, do not meet the resources circulation pattern of conservation-minded society.
Similarly, along with deepening continuously of modernization, the cobalt product that smelting process is produced obtains application more and more widely, for example: materials such as the samarium-cobalt alloy in the magneticsubstance, nickel cobalt (alloy), the hydrogen storage alloy of being made up of rare earth element/cobalt and nickel element and various cobalt-base alloy steel ...Making in the melting mode in the process of cobalt product, must use the cobalt metal sheet as cobalt additive; And the cobalt sheet still is a kind of catalyst of having many uses.This shows that the demand of cobalt metal sheet is also increasing.
Similarly, in the prior art, the method for producing the cobalt metal sheet also is an electrolytic process.Normally make thick cobalt anode as raw material with nickel electrowinning cobalt slag or pyrite cinder etc., obtain electrolytic cobalt through dissolving anode electrolysis method at negative electrode, perhaps make refining cobalt chloride solution, on negative electrode, obtain electrolytic cobalt through the galvanic deposit of insoluble anode electrolytic process cobalt with above-mentioned raw materials.Then electrolytic cobalt is scraped from negative electrode and form the cobalt sheet.Electrolysis legal system cobalt sheet can obtain the very high cobalt sheet of purity, and obviously, the energy consumption of electrolysis legal system cobalt is also very high, and is also quite serious to the pollution of environment.
On the other hand, along with various discarded electrical equipment, discarded industry or civil goods increase, nickel wherein, cobalt waste material are also increasing, and not only contaminate environment also causes the wasting of resources.
Therefore, if can be raw material with nickel, cobalt waste material, adopt non-electrolytic environment-friendly method to produce nickel, cobalt raw material cheaply, will be the important channel that alleviation nickel, cobalt resource are in short supply, innovate nickel, the cobalt mode of production.
Summary of the invention
Above-mentioned shortcoming at prior art, the objective of the invention is to provide a kind of eco-friendly nickel/cobalt/iron alloy production technique and system, this technology and device systems have following advantage: with useless nickel, cobalt is raw material, adopt energy-saving consumption-reducing, eco-friendly method to produce nickel/cobalt/iron alloy, the alternative pure nickel plate of product, cobalt sheet are for alloy industries such as stainless steel provide nickel/cobalt/iron master alloy cheaply.
For this reason, one of technical solution of the present invention is a kind of eco-friendly nickel/cobalt/iron alloy production technique, this production technique comprises the steps: A) in smelting furnace, feeding under the oxygen-containing gas condition, to contain the raw material of ferrophosphorus and the waste material or the material mixing melting of nickeliferous and/or cobalt and obtain mixed melting liquid, make nickel and/or the cobalt that phosphorus combustion heat supplying in the raw material, the iron in the raw material are simple substance attitude or lower valency as reductive agent with the nickel and/or the cobalt reduction reaction of oxidation state; B) keep feeding oxygen-containing gas, add slag former in mixed melting liquid, continue the reduction reaction of iron in the raw material, generating bigger nickel of less slag of proportion and proportion and/or ferro-cobalt is main nickel and/or ferro-cobalt fused solution; C) slag is discharged from the smelting furnace middle part, nickel and/or ferro-cobalt fused solution are derived from the smelting furnace bottom; D) nickel and/or ferro-cobalt fused solution are obtained nickel/cobalt/iron alloy through quick cooling.
Technology of the present invention, according to the analysis of exploration, with a unique view the discovery, in the iron phosphorus waste residue that the smelting furnace of refinement phosphorus product is discharged, make phosphorus be in to go back ortho states or zero-valent state owing to the electronegativity of phosphorus is better than iron, but and be in the phosphorus of going back ortho states or zero-valent state and suitably be easy to be volatilized and and metal separation under the high temperature by oxygen institute's oxidation.This rule of process makes full use of the present invention, phosphorus in the iron phosphorus waste residue that the smelting furnace of employing refinement phosphorus product is discharged is fuel, waste material or the material that contains cobalt and/or nickel comprised that the electric core material in the depleted chemical power source is carried out high temperature melting in the modern society, not only made full use of phosphorus fuel thermal energy, but also realized the separation of phosphorus; And, under the condition of high temperature, except allowing volatile metals such as wherein zinc, cadmium be volatilized, so that outside collecting by special gathering system, what technology of the present invention was also utilized under the condition of high temperature iron in the iron phosphorus waste residue generates permivar phase or Rhometal phase or ferro-cobalt phase than strong reducing property with nickel in the waste material and/or cobalt reduction; Can contain the silicon-dioxide sand by interpolation then is main slag former, make in the waste material impurity such as calcium magnalium generate low-gravity slag phase, thereby the high temperature that reaches cobalt nickel and foreign metal separates.Technology of the present invention, comprehensively, utilized above-mentioned a series of law discovery dexterously, realized with useless nickel, cobalt be raw material, the purpose of producing nickel/cobalt/iron alloy with energy-saving consumption-reducing, eco-friendly mode, the alternative pure nickel plate of the product that makes, cobalt sheet are for alloy industries such as stainless steel provide nickel/cobalt/iron master alloy cheaply.
By last process mechanism analysis as seen, technology of the present invention is a kind of energy-conserving and emission-cutting technology of innovation, and very friendly to environment: at first, technology of the present invention need not consume fuel such as electricity, coal, coke or oil, Sweet natural gas, but be fuel by the phosphorus in the iron phosphorus slag, for pyroprocess provides thermal source; Secondly, utilize iron in the iron phosphorus slag as reductive agent and alloying constituent, with cobalt or nickel that the cobalt or the nickel of oxidation state is reduced into simple substance, simultaneously, iron is at high temperature produced permivar or Rhometal or ferro-cobalt mutually as alloying constituent with cobalt nickel.The alternative pure nickel plate of nickel/cobalt of the present invention/iron alloy product, cobalt sheet, as the nickel and/or the ferro-cobalt master alloy of metallurgy industries such as stainless steel, and cost is lower.
Technology of the present invention can make full use of in original metallurgy or the phosphorus product industry in a large number can only landfill disposal the iron phosphorus slag as raw material, can make full use of in the modern society discarded in a large number again, electric core material with chemical power source of huge latency environment harm, two kinds of a large amount of waste materials that exist are transformed into the starting material that modern society is badly in need of, nickeliferous and/or cobalt waste material of the present invention, mainly from nickeliferous ni-mh, the NI-G old and useless battery, disused mobile battery of perhaps nickeliferous and/or cobalt etc., show through initial analysis: technology of the present invention can be with nickeliferous and/or cobalt waste material from nickel content 10%, or contain cobalt amount 10%, be purified to the nickel cobalt contents greater than more than 60%.
By last analysis as seen, the present invention also be a low ore grade nickel and/or cobalt raw material the high temperature purification process promptly: at high temperature by constantly adding low-grade nickel and/or cobalt raw material, constantly slag making despumation, nickel and/or cobalt contents improve constantly in the alloy of producing, finally, when nickel or cobalt or nickel cobalt contents are above greater than 30%, typically greater than 60% the time, make the master alloy product.Pure Rhometal is used for stainless steel industry, the iron alloy of nickel cobalt or ferro-cobalt, be used for the higher-grade raw material that the nickel cobalt is smelted, can reduce the consumption of chemical feedstocks, shorten purification schemes: because low grade material is when carrying out chemical purification, need to consume a large amount of chemical reagent, impurity is dissolved together, separate then, long flow path, consumption are greatly; And the present invention can not consume chemical reagent, effectively separating impurity, upgrade.
Technology of the present invention also comprises following concrete improvement:
For reaction conditions in the better control smelting furnace, described steps A) before, also comprise steps A 1): by suitable proportion, phosphorous iron material, waste material or material nickeliferous and/or cobalt that shape is regardless of add from smelting furnace middle part charging opening respectively or simultaneously; Perhaps that the waste material or the material of phosphorous iron material, nickeliferous and/or cobalt is broken in advance, and mix by suitable proportion, obtain even-grained mixture charge after, add from smelting furnace middle part charging opening again.
For energy-conservation and keep good production efficiency, described steps A 1), B), C), D) carry out described steps A intermittently relatively) carry out continuously relatively.
For reaction conditions in the better control smelting furnace, in described steps A 1) in, the ratio of controlling phosphorus in the described mixture charge is 5-50 (wt%); Phosphorus in the described ferrophosphorus raw material and iron mainly are simple substance attitude or sub-compound state; Described waste material or material nickeliferous and/or cobalt are compound state or metallic state.
In described steps A), B) in, the temperature of controlling described reduction reaction is 700-1600 ℃ of scope.
In order fully to guarantee to react completely in the smelting furnace described reduction reaction process continuity 10-360 hour according to the working of a furnace.
The element ratio of considering fusion nickel/cobalt/iron alloy may be in the amorphous phase, for guaranteeing that melting obtains nickel/cobalt/iron alloy product and has better physics and chemistry state, among the described step D, the quick cooling of described nickel and/or ferro-cobalt fused solution is to carry out on the metal roller of uniform rotation.
Described slag former is principal constituent with the silicon oxide.Technology of the present invention by adding cheap sand, generates stable slag phase to oxide compounds such as the calcium in the waste material, magnesium, thereby realizes alloy phase and slag separating mutually.Therefore, realized energy-saving consumption-reducing, reduced product cost.
Reaction in the smelting furnace of the present invention is specific as follows:
Total chemical reaction:
Divide the chemistry reaction:
P+O
2→ → P
2O
5+ Δ H (heat),
Fe+O
2→→Fe
2O
3，
CoxOy(NiO)+Fe→→Co(Ni)，
SiO
2+P
2O
5+Fe
2O
3+CaO+MgO+MnO→→SiO
2-P
2O
5-Fe
2O
3-CaO-MgO-MnO。
In order to guarantee environmental friendliness to greatest extent, described production technique comprises that also flue gas passes through dedusting, cooling is reclaimed and contained cadmium, zinc powder with drawing in the described smelting furnace, will reclaim phosphorus oxide, sulfur oxide gas with solution absorption through dedusting, refrigerative Purge gas again.
Another correlation technique solution of the present invention is a kind of production system that is used for eco-friendly as mentioned above nickel/cobalt/iron alloy production technique, described production system comprises smelting furnace, the metal roller water cooler, smelting furnace comprises and is separately positioned on top among it, the charging opening of middle and lower part, slag notch, contain the oblique smelting furnace middle and lower part that enters of the oxygen air blast mouth of pipe, above space, the middle part of described smelting furnace is the solid-holding space, be provided with the fused solution outlet in described smelting furnace bottom, the top of described smelting furnace is provided with flue, and described metal roller water cooler correspondence is installed in the fused solution exit of described smelting furnace bottom.
Production system of the present invention, can guarantee that with useless nickel, phosphorus product slag be raw material, adopt energy-saving consumption-reducing, eco-friendly method to produce crystal formation or armorphous nickel/cobalt/iron alloy, product can be alloy industry such as stainless steel nickel/cobalt/iron master alloy cheaply is provided.
In order further to reclaim useful resources, to reduce environmental pollution, production system of the present invention also comprises cooling particle collector and tail gas absorber, and described cooling particle collector is connected with described smelting furnace top flue by pipeline with tail gas absorber.
The invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the structural representation block diagram of production system embodiment of the present invention.
Embodiment
Production system embodiment:
As Fig. 1, be depicted as the structural representation block diagram of production system embodiment of the present invention.It comprises smelting furnace 1O, metal roller water cooler 20, cooling particle collector 30 and tail gas absorber 40, smelting furnace charging opening 11, slag notch 12 are separately positioned on middle and upper part, the middle and lower part of described smelting furnace 10, contain the oxygen air blast mouth of pipe 13 oblique smelting furnace middle and lower parts that enter, above space, the middle part of described smelting furnace is the solid-holding space, its volume and highly account for the smelting furnace cumulative volume and highly 2/3.Described metal roller water cooler 40 correspondences are installed in the fused solution exit 14 of described smelting furnace 10 bottoms, described cooling particle collector 30 is connected by the flue 15 of pipeline with described smelting furnace 10 tops with tail gas absorber 40, the collector 31 of cooling particle collector 30 is collected reuse with the metallic dust in the flue gas (dotted line is represented), the alkaline absorption solution groove 41 usefulness alkali lye of tail gas absorber 40 generate salt with acid tail gas, concentrate the back reuse of purifying.
Production technique embodiment:
Eco-friendly nickel/the cobalt of the present invention/iron alloy production technique is carried out in as the production system embodiment of Fig. 1, and it comprises the steps:
Steps A 1): the waste material or the material of phosphorous iron material, nickeliferous and/or cobalt is broken in advance, and mix by suitable proportion, obtain even-grained mixture charge after, add from smelting furnace middle part charging opening again.In this steps A 1) in, the ratio of controlling phosphorus in the described mixture charge is S; Phosphorus in the described ferrophosphorus raw material and iron mainly are simple substance attitude or sub-compound state; Described waste material or material nickeliferous and/or cobalt are compound state or metallic state.
A) in smelting furnace, feeding under the oxygen-containing gas condition, will contain the raw material of ferrophosphorus and the waste material or the material mixing melting of nickeliferous and/or cobalt and obtain mixed melting liquid, the temperature of controlling described reduction reaction is in the T1 scope.Make nickel and/or the cobalt that phosphorus combustion heat supplying in the raw material, the iron in the raw material are simple substance attitude or lower valency as reductive agent with the nickel and/or the cobalt reduction reaction of oxidation state;
B) keep feeding oxygen-containing gas, the temperature of control reduction reaction is in the T2 scope.Adding with the silicon oxide in mixed melting liquid is the slag former of principal constituent, continues the reduction reaction of iron in the raw material, and generating bigger nickel of less slag of proportion and proportion and/or ferro-cobalt is main nickel and/or ferro-cobalt fused solution;
In described steps A), B) in, whole reduction reaction process continuity U hour.
C) stop to lead to oxygen, stopping the reduction reaction process, slag is discharged from the smelting furnace middle part, nickel and/or ferro-cobalt fused solution are derived from the smelting furnace bottom;
D) metal roller with nickel and/or the uniform rotation of ferro-cobalt fused solution process carries out quick cooling, obtains nickel/cobalt/iron alloy.
Described production technique comprises that also gas is drawn on described smelting furnace top contains cadmium, zinc powder through dedusting, cooling recovery, will reclaim phosphorus oxide, sulfur oxide gas with solution absorption through dedusting, refrigerative Purge gas again.
The main control parameters of production technique series embodiment of the present invention and the nickel ferro-cobalt master alloy product that makes see following table 1 for details:
Table 1
As seen from the above table: production technique of the present invention can be produced near the required permivar in market, need only further refine or be added directly in the smelting furnace just can make the commercial alloys product.
Claims (10)
1. eco-friendly nickel/cobalt/iron alloy production technique, this production technique comprises the steps: A) in smelting furnace, feeding under the oxygen-containing gas condition, to contain the raw material of ferrophosphorus and the waste material or the material mixing melting of nickeliferous and/or cobalt and obtain mixed melting liquid, make nickel and/or the cobalt that phosphorus combustion heat supplying in the raw material, the iron in the raw material are simple substance attitude or lower valency as reductive agent with the nickel and/or the cobalt reduction reaction of oxidation state; B) keep feeding oxygen-containing gas, add slag former in mixed melting liquid, continue the reduction reaction of iron in the raw material, generating bigger nickel of less slag of proportion and proportion and/or ferro-cobalt is main nickel and/or ferro-cobalt fused solution; C) slag is discharged from the smelting furnace middle part, nickel and/or ferro-cobalt fused solution are derived from the smelting furnace bottom; D) nickel and/or ferro-cobalt fused solution are obtained nickel/cobalt/iron alloy through quick cooling.
2. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique, it is characterized in that: described steps A) before, also comprise steps A 1): by suitable proportion, phosphorous iron material, waste material or material nickeliferous and/or cobalt that shape is regardless of add from smelting furnace middle part charging opening respectively or simultaneously; Perhaps that the waste material or the material of phosphorous iron material, nickeliferous and/or cobalt is broken in advance, and mix by suitable proportion, obtain even-grained mixture charge after, add from smelting furnace middle part charging opening again.
3. eco-friendly nickel/cobalt as claimed in claim 2/iron alloy production technique is characterized in that: in described steps A 1) in, the ratio of controlling phosphorus in the described mixture charge is 5-50 (wt%); Phosphorus in the described ferrophosphorus raw material and iron mainly are simple substance attitude or sub-compound state; Described waste material or material nickeliferous and/or cobalt are compound state or metallic state.
4. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique is characterized in that: in described steps A), B) in, the temperature of controlling described reduction reaction is 700-1600 ℃ of scope.
5. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique is characterized in that: described reduction reaction process continuity 10-360 hour.
6. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique is characterized in that: among the described step D, the quick cooling of nickel and/or ferro-cobalt fused solution is to carry out on the metal roller of uniform rotation.
7. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique is characterized in that: described slag former is principal constituent with the silicon oxide.
8. eco-friendly nickel/cobalt as claimed in claim 1/iron alloy production technique, it is characterized in that: described production technique comprises that also flue gas passes through dedusting, cooling is reclaimed and contained cadmium, zinc powder with drawing in the described smelting furnace, will reclaim phosphorus oxide, sulfur oxide gas with solution absorption through dedusting, refrigerative Purge gas again.
9. eco-friendly nickel/cobalt/iron alloy production system that is used for claim 1-8 production technique, it comprises smelting furnace, smelting furnace comprises and is separately positioned on top among it, the charging opening of middle and lower part, slag notch, contain the oblique smelting furnace middle and lower part that enters of the oxygen air blast mouth of pipe, above space, the middle part of described smelting furnace is the solid-holding space, be provided with the fused solution outlet in described smelting furnace bottom, the top of described smelting furnace is provided with flue, it is characterized in that: described production system also comprises the metal roller water cooler, and described metal roller water cooler correspondence is installed in the fused solution exit of described smelting furnace bottom.
10. as eco-friendly nickel/cobalt/iron alloy production system as described in the claim 9, it is characterized in that: described production system also comprises cooling particle collector and tail gas absorber, and described cooling particle collector is connected with described smelting furnace top flue by pipeline with tail gas absorber.
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| CN102492847B (en) * | 2011-12-14 | 2013-07-31 | 中航上大金属再生科技有限公司 | Method for smelting intermediate alloy by utilizing waste nickel powder |
| CN105331830A (en) * | 2015-11-30 | 2016-02-17 | 钱国庆 | Furnace for smelting ferro-nickel |
| CN114657401A (en) * | 2022-03-15 | 2022-06-24 | 金川镍钴研究设计院有限责任公司 | Production method of 4J29 alloy |
| CN114875245A (en) * | 2022-05-30 | 2022-08-09 | 金川镍钴研究设计院有限责任公司 | Method for producing 4J29 alloy raw material from nickel-cobalt slag |
| CN115233013A (en) * | 2022-07-19 | 2022-10-25 | 西安聚能高温合金材料科技有限公司 | Preparation method of difficult-deformation high-temperature alloy GH4141 alloy ingot |
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Effective date of registration: 20110826 Address after: 448124 Jingmen high tech Industrial Development Zone, Jingmen, Hubei Patentee after: Jingmen GEM New Material Co., Ltd. Address before: 518104, Shenzhen, Guangdong Province, Baoan District, Sha Wu Town, West Industrial Zone, No. 50 Patentee before: Shenzhen GEM High-tech Co., Ltd. |