CN113025819A - Method for recycling spectrum pure graphite crucible - Google Patents

Method for recycling spectrum pure graphite crucible Download PDF

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Publication number
CN113025819A
CN113025819A CN202110209230.9A CN202110209230A CN113025819A CN 113025819 A CN113025819 A CN 113025819A CN 202110209230 A CN202110209230 A CN 202110209230A CN 113025819 A CN113025819 A CN 113025819A
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China
Prior art keywords
graphite crucible
pure graphite
recycling
metal
melting
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Pending
Application number
CN202110209230.9A
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Chinese (zh)
Inventor
冯兆龙
冯远超
郑帮智
唐新新
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Priority to CN202110209230.9A priority Critical patent/CN113025819A/en
Publication of CN113025819A publication Critical patent/CN113025819A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/06Alloys
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/0025Adding carbon material
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/08Apparatus
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04Refining by applying a vacuum
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention relates to a recycling method of a spectral pure graphite crucible, in particular to a method for using a used spectral pure graphite crucible for vacuum induction melting of steel. The invention solves the technical problem of providing a recycling method of a spectral pure graphite crucible. The method comprises the following steps: putting other raw materials except the spectral pure graphite crucible and the active metal into a vacuum induction smelting furnace, vacuumizing, electrically melting, filling argon after melting down, then adding the pretreated spectral pure graphite crucible and the active metal, continuously smelting to obtain molten steel, and casting the molten steel into ingots. The method uses the recycled spectral pure graphite crucible as a carbon material to carry out steel vacuum induction smelting, can accurately control the carbon content of the alloy, and realizes the reutilization of waste materials.

Description

Method for recycling spectrum pure graphite crucible
Technical Field
The invention relates to a recycling method of a spectral pure graphite crucible, in particular to a method for using a used spectral pure graphite crucible for vacuum induction melting of steel.
Background
The spectral pure graphite is high-purity graphite applied to the fields of emission spectrum, atomic absorption spectrum, infrared absorption spectrum, gas analysis and the like, is very pure, does not contain impurities which can damage other element analysis except carbon elements, and has the total ash content of 20 multiplied by 10-6The following. The graphite has high purity requirement, so the unit price is high. Meanwhile, after the sample is analyzed each time, the sample needs to be melted at high temperature and then analyzed, and the metal cannot be completely removed after cooling, so that the spectral pure graphite crucible is disposable so as to prevent the analysis result from being influenced after being repeatedly used. Because the garbage can not be reused, the garbage can only be treated as garbage after being used.
In order to ensure the performance of the steel material, the lower the carbon content is, the better the carbon content is, and sometimes a certain amount of carbon needs to be added to ensure the comprehensive mechanical properties of the steel material. The conventional method is to carry out the recarburization by iron alloy or ordinary graphite. Because the iron alloy or the common graphite carries other impurities such as sulfur and phosphorus in the iron alloy, ash in the common graphite and the like while being carburized. The method has the advantages that the used spectrally pure graphite crucible is simply treated and then is used as carbon element to be added when steel is smelted in the vacuum induction smelting furnace, so that the purpose of accurately controlling the carbon content can be achieved, meanwhile, other impurity elements cannot be added, the purity of molten steel is guaranteed, and the recycling of the spectrally pure graphite crucible is realized.
Disclosure of Invention
The invention aims to solve the problems that the spectral pure graphite crucible used after chemical analysis has no utilization value, can only be treated as waste and pollutes the environment.
In view of the above object, the present invention provides a method for recycling a spectrally pure graphite crucible, comprising the steps of: putting other raw materials except the spectral pure graphite crucible and the active metal into a vacuum induction smelting furnace, vacuumizing, electrically melting, filling argon after melting down, then adding the pretreated spectral pure graphite crucible and the active metal, continuously smelting to obtain molten steel, and casting the molten steel into ingots.
In the above method of recycling the spectrally pure graphite crucible, the spectrally pure graphite crucible is a crucible used when a chemical element is analyzed by gas analysis, emission spectroscopy, infrared absorption spectroscopy, or atomic absorption spectroscopy.
Preferably, in the method of recycling a spectrally pure graphite crucible, the spectrally pure graphite crucible is a crucible used for analyzing a chemical element by a melting-infrared absorption method.
In the recycling method of the spectrally pure graphite crucible, the pretreated spectrally pure graphite crucible is separated by a mechanical method, so that the spectrally pure graphite crucible without residual metal is obtained.
Wherein, in the recycling method of the spectral pure graphite crucible, the vacuum degree is less than 10 Pa.
In the method for recycling the spectrally pure graphite crucible, the electric melting is electric induction heating.
In the method for recycling the spectrally pure graphite crucible, the meltdown means that no solid exists in the crucible of the vacuum induction melting furnace.
In the method for recycling the spectrally pure graphite crucible, the active metal is at least one of metal silicon, metal manganese, metal aluminum, metal titanium, metal magnesium and rare earth.
In the recycling method of the spectrally pure graphite crucible, the purity of the argon gas is more than 99.9%.
In the recycling method of the spectral pure graphite crucible, argon is filled into the furnace for 0.3-0.6 atmospheric pressure.
The method comprises the steps of treating the spectral pure graphite crucible used for chemical analysis in a mechanical mode, and adding the spectral pure graphite crucible into a vacuum induction smelting furnace in a mode of a recarburizing raw material, so that the accurate control of carbon elements is realized when the alloy is subjected to vacuum induction smelting, and the waste can be reused.
Detailed Description
The invention provides a recycling method of a spectral pure graphite crucible, which comprises the following steps:
A. pretreating a spectral pure graphite crucible: separating by a mechanical method to obtain a crucible without residual metal; the spectral pure graphite crucible is used for analyzing chemical elements by gas analysis, emission spectrum, infrared absorption spectrum or atomic absorption spectrum; preferably, the spectrally pure graphite crucible is used for analyzing chemical elements by a melting-infrared absorption method;
B. putting clean and dry raw materials except the pretreated spectrally pure graphite crucible and the active metal into a crucible of a vacuum induction melting furnace, and putting the pretreated spectrally pure graphite crucible and the active metal into a hopper; the active metal is at least one of metal silicon, metal manganese, metal aluminum, metal titanium, metal magnesium and rare earth;
C. closing the furnace cover, starting the mechanical pump and the Roots pump, enabling the vacuum degree in the furnace to be less than 10Pa, and then transmitting power, and melting other raw materials except the pretreated spectral pure graphite crucible and the active metal in the crucible through electric induction heating until no solid exists in the crucible of the vacuum induction melting furnace;
D. stopping vacuum filling, filling argon with the purity of more than 99.9 percent to ensure that the air pressure in the furnace is 0.3-0.6 atmospheric pressure, and sequentially adding the pretreated spectral pure graphite crucible and active metal into a hopper;
E. and pouring molten steel into the steel ingot mold by adopting a direct pouring mode.
Because the activity of the active metal is higher, other raw materials except the pretreated spectral pure graphite crucible and the active metal need to be melted down, and the active metal is added under the protective atmosphere, so that the reaction between the active metal and oxygen is prevented, and the alloy components are reduced; meanwhile, carbon dioxide and nitrogen also influence molten steel in the smelting process, and argon is used as the cheapest inert gas, has better economical efficiency, does not react with the molten steel, is an ideal protective gas for vacuum smelting, and is introduced as the protective gas.
The following examples are given to further illustrate the embodiments of the present invention, but are not intended to limit the scope of the present invention to the examples.
Example 1
Preparing GH4169 steel ingots:
A. pretreating a spectral pure graphite crucible used when chemical elements are analyzed by a melting-infrared absorption method, and mixing alloy components and the pretreated spectral pure graphite crucible according to the proportion of 0.012 wt% of carbon content;
B. putting clean and dry metal chromium, electrolytic nickel, metal molybdenum, pure iron and metal niobium into a crucible of a vacuum induction smelting furnace, and putting a pretreated spectral pure graphite crucible, metal silicon, metal manganese, metal aluminum and metal titanium into a hopper;
C. closing the furnace cover, starting the mechanical pump and the Roots pump, transmitting power when the vacuum degree in the furnace is less than 10Pa, and melting the furnace charge in the crucible by electric induction heating until no solid exists in the crucible of the vacuum induction melting furnace;
D. stopping vacuum filling, filling argon gas with the pressure of 0.3-0.6 atm, and sequentially adding the spectral pure graphite crucible, the metal silicon, the metal manganese, the metal aluminum and the metal titanium which are treated in the hopper;
E. and pouring molten steel into the steel ingot mold by adopting a direct pouring mode.
After sampling and chemical analysis, the carbon content in the steel ingot is 0.011 wt%, which meets the smelting requirement.
Example 2
Preparing GH3625 steel ingots:
A. pretreating a spectral pure graphite crucible used when chemical elements are analyzed by a melting-infrared absorption method, and mixing alloy components and the pretreated spectral pure graphite crucible according to the proportion of 0.010 wt% of carbon content;
B. putting clean and dry metal chromium, electrolytic nickel, metal molybdenum and metal niobium into a crucible of a vacuum induction smelting furnace, and putting a pretreated spectral pure graphite crucible, metal silicon, metal manganese, metal aluminum and metal titanium into a hopper;
C. closing the furnace cover, starting the mechanical pump and the Roots pump, transmitting power when the vacuum degree in the furnace is less than 10Pa, and melting the furnace charge in the crucible by electric induction heating until no solid exists in the crucible of the vacuum induction melting furnace;
D. stopping vacuum filling, filling argon gas with the pressure of 0.3-0.6 atm, and sequentially adding the processed spectrally pure graphite crucible, metal silicon, metal manganese, metal aluminum and metal titanium through a hopper;
E. pouring molten steel into the steel ingot mold by adopting a direct pouring mode;
after sampling and chemical analysis, the carbon content in the steel ingot is 0.0098 wt%, which meets the smelting requirement.
In the processes of preparing steel ingots in the embodiments 1 and 2, the recycled spectrally pure graphite crucible is used, so that the purpose of accurately controlling the carbon content is achieved, and most importantly, the spectrally pure graphite crucible is recycled, so that the cost is saved, and the hidden danger of environmental pollution caused by the waste spectrally pure graphite crucible is eliminated.

Claims (9)

1. The recycling method of the spectral pure graphite crucible is characterized by comprising the following steps: the method comprises the following steps: putting other raw materials except the spectral pure graphite crucible and the active metal into a vacuum induction smelting furnace, vacuumizing, electrically melting, filling argon after melting down, then adding the pretreated spectral pure graphite crucible and the active metal, continuously smelting to obtain molten steel, and casting the molten steel into ingots.
2. The method of recycling a spectrally pure graphite crucible according to claim 1, characterized in that: the spectral pure graphite crucible is used for analyzing chemical elements by gas analysis, emission spectrum, infrared absorption spectrum or atomic absorption spectrum; preferably, the spectrally pure graphite crucible is a crucible used for analyzing a chemical element by a melting-infrared absorption method.
3. The method of recycling a spectrally pure graphite crucible according to claim 1 or 2, characterized in that: the pretreated spectrally pure graphite crucible is separated by a mechanical method, and the spectrally pure graphite crucible without residual metal is obtained.
4. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 3, characterized in that: the vacuum degree is less than 10 Pa.
5. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 4, characterized in that: the electric melting is electric induction heating.
6. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 5, characterized in that: the meltdown means that no solid exists in a crucible of the vacuum induction melting furnace.
7. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 6, characterized in that: the active metal is at least one of metal silicon, metal manganese, metal aluminum, metal titanium, metal magnesium and rare earth.
8. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 7, characterized in that: the purity of the argon gas is more than 99.9 percent.
9. The method of recycling a spectrally pure graphite crucible according to any one of claims 1 to 8, characterized in that: filling argon into the furnace to 0.3-0.6 atmospheric pressure.
CN202110209230.9A 2021-02-24 2021-02-24 Method for recycling spectrum pure graphite crucible Pending CN113025819A (en)

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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1624181A (en) * 2004-12-15 2005-06-08 宁波浙东精密铸造有限公司 Strongtough high gilicon cast steel and its manufacturing method
CN102851564A (en) * 2012-05-18 2013-01-02 中国科学院合肥物质科学研究院 Vacuum melting method of high-strength high-elongation alloy steel
CN103160726A (en) * 2013-03-04 2013-06-19 内蒙古包钢钢联股份有限公司 Carbon-iron alloy for recarburization and manufacture method thereof
KR20150068568A (en) * 2013-12-12 2015-06-22 이태수 Composition of silicone-carbon based thermic reducing agent and the manufacturing method thereof
CN105463298A (en) * 2015-12-01 2016-04-06 东北大学 Method for smelting low-aluminum high-nitrogen martensitic stainless steel in pressurization and induction manner
CN105970074A (en) * 2016-05-30 2016-09-28 河北钢铁股份有限公司 Method for quickly smelting low-nitrogen stainless steel through vacuum induction furnace
CN106756434A (en) * 2016-12-05 2017-05-31 东北大学 Low activation ferrite/martensite steel and its smelting process of oxide dispersion intensifying
CN107502818A (en) * 2017-08-08 2017-12-22 武钢集团昆明钢铁股份有限公司 A kind of anti-corrosion extraordinary forging steel of high intensity low density and preparation method thereof
CN109988971A (en) * 2019-04-16 2019-07-09 东北大学 A method of producing special ultra-pure high-speed tool steel
CN111020104A (en) * 2019-11-28 2020-04-17 马鞍山市弘信冶金材料有限公司 Production method of graphite carburant
CN111519108A (en) * 2020-06-09 2020-08-11 西安建筑科技大学 Zirconium-reinforced low-activation martensitic steel and preparation method thereof

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1624181A (en) * 2004-12-15 2005-06-08 宁波浙东精密铸造有限公司 Strongtough high gilicon cast steel and its manufacturing method
CN102851564A (en) * 2012-05-18 2013-01-02 中国科学院合肥物质科学研究院 Vacuum melting method of high-strength high-elongation alloy steel
CN103160726A (en) * 2013-03-04 2013-06-19 内蒙古包钢钢联股份有限公司 Carbon-iron alloy for recarburization and manufacture method thereof
KR20150068568A (en) * 2013-12-12 2015-06-22 이태수 Composition of silicone-carbon based thermic reducing agent and the manufacturing method thereof
CN105463298A (en) * 2015-12-01 2016-04-06 东北大学 Method for smelting low-aluminum high-nitrogen martensitic stainless steel in pressurization and induction manner
CN105970074A (en) * 2016-05-30 2016-09-28 河北钢铁股份有限公司 Method for quickly smelting low-nitrogen stainless steel through vacuum induction furnace
CN106756434A (en) * 2016-12-05 2017-05-31 东北大学 Low activation ferrite/martensite steel and its smelting process of oxide dispersion intensifying
CN107502818A (en) * 2017-08-08 2017-12-22 武钢集团昆明钢铁股份有限公司 A kind of anti-corrosion extraordinary forging steel of high intensity low density and preparation method thereof
CN109988971A (en) * 2019-04-16 2019-07-09 东北大学 A method of producing special ultra-pure high-speed tool steel
CN111020104A (en) * 2019-11-28 2020-04-17 马鞍山市弘信冶金材料有限公司 Production method of graphite carburant
CN111519108A (en) * 2020-06-09 2020-08-11 西安建筑科技大学 Zirconium-reinforced low-activation martensitic steel and preparation method thereof

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