CN111621642A - Method for recovering and purifying Nb sawdust residue - Google Patents
Method for recovering and purifying Nb sawdust residue Download PDFInfo
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- CN111621642A CN111621642A CN202010145545.7A CN202010145545A CN111621642A CN 111621642 A CN111621642 A CN 111621642A CN 202010145545 A CN202010145545 A CN 202010145545A CN 111621642 A CN111621642 A CN 111621642A
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- sawdust
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/003—Dry processes only remelting, e.g. of chips, borings, turnings; apparatus used therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
A method for recovering and purifying Nb sawdust residues comprises the following steps: adding HNO3And H2Completely covering the mixed solution of O on the surface of the Nb sawdust, soaking for more than 20 minutes, and then cleaning for a certain time by using normal-temperature water; after the Nb sawdust is spread, magnetic substances in the Nb sawdust are screened out through magnetic separation; dividing the Nb sawdust into a plurality of equal parts and pressing the equal parts into a plurality of parts with the density of more than 4g/cm3The electrode blocks are welded into an electrode meeting the requirements of the electron beam furnace horizontal feeding through a vacuum argon arc welding box; and purifying the electrode by an electron beam furnace to obtain the Nb ingot. Acid washing, magnetic material screening and electronAnd oil stain and impurities in the Nb sawdust are separated by purifying the beam furnace, and finally the Nb ingot is obtained, so that the problem of the same-grade recovery of the Nb sawdust is solved.
Description
Technical Field
The invention relates to the technical field of residue treatment and sawdust residue recovery, in particular to a method for recovering and purifying Nb sawdust residues.
Background
Nb is an important zirconium alloy additive element and has a large addition proportion; meanwhile, as the melting point of the Nb element is higher, in order to prevent Nb from forming unmelted inclusion in the zirconium matrix, the Nb metal has requirements on the size when being added, and Nb ingots are required to be sawed and planed into Nb scraps for use. About 6% of sawdust is generated in the sawing process, so that Nb waste is caused; meanwhile, the saw dust is mixed with foreign matters such as a saw machine abrasion tool bit, a stainless steel brush, oil stains, cutting fluid and the like. In the co-line production of various metals, if the metals of different types are thoroughly cleaned according to the particularity of the sawing machine, the production cost is high, and the grade-distinguished sawing operation is not carried out in the general industrial production, so that a large amount of other metals are mixed in the recycled Nb sawdust, and the sawdust can only be treated as waste. The cost of Nb is high, about 1000 yuan/kg, which results in energy waste.
Disclosure of Invention
Objects of the invention
The invention aims to provide a method for recovering and purifying residual Nb sawdust.
(II) technical scheme
To solve the above problems, according to one aspect of the present invention, there is provided a method for recovering Nb sawdust residue and an Nb sawdust recycling apparatusA method of purification comprising: adding HNO3And H2Completely covering the mixed solution of O on the surface of the Nb sawdust, soaking for more than 20 minutes, and then cleaning for a certain time by using normal-temperature water; after the Nb sawdust is spread, magnetic substances in the Nb sawdust are screened out through magnetic separation; dividing the Nb sawdust into a plurality of equal parts and pressing the equal parts into a plurality of parts with the density of more than 4g/cm3The electrode blocks are welded into an electrode meeting the requirements of the electron beam furnace horizontal feeding through a vacuum argon arc welding box; and purifying the electrode by an electron beam furnace to obtain the Nb ingot.
Further, weld into the electrode that satisfies the horizontal feeding requirement of electron beam stove through vacuum argon arc welding case with a plurality of electrode blocks includes: before a plurality of electrode blocks are placed in a vacuum argon arc welding box for welding, the vacuum density of the vacuum argon arc welding box is kept to be less than or equal to 3Pa, the gas leakage rate of the vacuum argon arc welding box is kept to be less than or equal to 0.65Pa/min, and the welding current of the vacuum argon arc welding box is between 100A and 300A.
Further, the purification of the electrode by an electron beam furnace to obtain the Nb ingot comprises the following steps: the electrode is loaded into a bin of the electron beam furnace in a transverse feeding mode; sealing the electron beam furnace and vacuumizing to ensure that the vacuum density is less than or equal to 3Pa, and adjusting the air leakage rate of the electron beam furnace to be less than or equal to 0.65 Pa/min; smelting the electrode by using an electron gun of an electron beam furnace to obtain Nb liquid drops; and injecting Nb liquid drops into a mold in a cooling system of the electron beam furnace for cooling to obtain Nb ingots.
Furthermore, the melting rate of the electron gun is 16-60kg/h, and the melting power of the electron gun is 104-156 KW.
Furthermore, the cooling time of the cooling system is more than or equal to 240 min.
Further, HNO3And H2In a mixed solution of O, HNO3：H2The volume ratio of O is 3: 1.
Further, before the magnetic separation screening, the method further comprises the following steps: the content of C element in Nb sawdust was analyzed.
Further, the time for cleaning with normal temperature water is more than five minutes.
Furthermore, the spreading thickness of the Nb sawdust is less than 50 mm.
(III) advantageous effects
The technical scheme of the invention has the following beneficial technical effects:
the process of treatment and recovery of the Nb sawdust residues is determined, and oil stains and cutting fluid on the surface of the Nb sawdust are removed by a surface treatment technology; the Nb filings mixed with a large amount of other metals are purified by an electron beam purification technology.
The situation that Nb sawdust generated in industrial production is treated as waste is changed, the Nb sawdust is recycled at the same level, waste is changed into valuable, the Nb sawdust can be directly used as intermediate alloy for product production after being processed, and precious metal resources are greatly saved.
Drawings
FIG. 1 is a flow chart of the steps of the method of recovering and purifying Nb sawdust residue provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Fig. 1 is a flow chart showing the steps of the method for recovering and purifying the Nb sawdust residue according to the present invention, and please refer to fig. 1. In one embodiment, the invention provides a method for recovering and purifying Nb sawdust residues, which comprises the following steps:
the method comprises the following steps: adding HNO3And H2And completely covering the mixed solution of O on the surface of the Nb sawdust, soaking for more than 20 minutes, and then cleaning for a certain time by using normal-temperature water.
Step two: and after the Nb sawdust is spread, magnetic substances in the Nb sawdust are screened out through magnetic separation.
Step three: dividing the Nb sawdust into a plurality of equal parts and pressing the equal parts into a plurality of parts with the density of more than 4g/cm3The electrode blocks are welded into a shape meeting the requirement by a vacuum argon arc welding boxThe electron beam furnace is provided with electrodes required by horizontal feeding.
Step four: and purifying the electrode by an electron beam furnace to obtain the Nb ingot.
Specifically, the Nb sawdust has a large specific surface area, emulsion is seriously polluted, the storage time is long, the specification is small, and the effect of using the alkaline degreasing agent is not obvious. Therefore, preferably, HNO is used3And H2The mixed acid solution of O completely covers the Nb chips and is applied to HNO3And H2In a mixed solution of O, HNO3：H2The volume ratio of O is 3: 1.
And HNO3And H2The mixed acid liquor of O soaks the Nb crumbs for more than 20 minutes, so that a certain removal amount is ensured, and oil stains can be effectively removed.
Optionally, the acid soak is followed by a more than five minute wash with warm water at ambient temperature.
Generally, scrap-shaped recovered scraps need to be cleaned by using an oil removal agent or a cleaning agent in special cleaning equipment after the scrap is crushed to a certain specification by using a crushing mechanism. And because the Nb sawdust has the characteristics of small size, interweaving into a mass and strong plasticity when being recycled, if the Nb sawdust is crushed and then cleaned, most of small scraps can run off along with water, and meanwhile, the Nb sawdust can be filled into gaps of equipment to damage the equipment. Therefore, the method is firstly cleaned and then pressed into the electrode block.
Optionally, the Nb sawdust needs to be dried after cleaning, so as to ensure that the subsequent process of preparing the electrode block is smoothly carried out.
Optionally, before the magnetic separation screening, the method further comprises: and analyzing the content of the C element in the Nb sawdust to ensure that the content of the C element at the moment is consistent with the control requirement of the content of the C element in the original Nb ingot. Is beneficial to subsequent purification.
Specifically, in step two, the cleaned Nb sawdust needs to be firstly tiled on a workbench, and the thickness of the tiled Nb sawdust is kept to be less than 50 mm. The thicker Nb sawdust layer makes the subsequent magnetic separation operation ineffective.
Optionally, in step three, the sawdust is divided into several equal parts by using an oil press and then pressed into electrode blocks of 50 × 50 × 500 mm.
In one embodiment, welding a plurality of electrode blocks into an electrode meeting the feeding requirement of the electron beam furnace through a vacuum argon arc welding box comprises the following steps: before a plurality of electrode blocks are placed in a vacuum argon arc welding box for welding, the vacuum density of the vacuum argon arc welding box is kept to be less than or equal to 3Pa, the gas leakage rate of the vacuum argon arc welding box is kept to be less than or equal to 0.65Pa/min, and the welding current of the vacuum argon arc welding box is between 100A and 300A.
In particular, the Nb sawdust has the characteristics of serious pollution and small specification, and is not easy to form. The phenomena of material falling and layering are serious after pressing by an oil press, and the strength of the Nb sawdust cannot meet the requirement of a vacuum consumable electrode. The purification capacity of the electron beam furnace is high, most of metal impurities in the Nb substrate can be purified in the electron beam furnace according to metal characteristics, the requirement on the electrode strength is not high due to the smelting mode of transverse feeding of the electron beam furnace, and Nb sawdust can be smelted in the furnace only by simple forming.
Optionally, the purifying the electrode by an electron beam furnace to obtain the Nb ingot comprises: the electrode is loaded into a bin of the electron beam furnace in a transverse feeding mode; sealing the electron beam furnace and vacuumizing to ensure that the vacuum density is less than or equal to 3Pa, and adjusting the air leakage rate of the electron beam furnace to be less than or equal to 0.65 Pa/min; smelting the electrode by using an electron gun of an electron beam furnace to obtain Nb liquid drops; and injecting Nb liquid drops into a mold in a cooling system of the electron beam furnace for cooling to obtain Nb ingots.
Specifically, an electron gun of the electron beam furnace directly strikes an electrode, and the electrode is heated and melted into droplets to realize purification, so that Nb droplets are obtained. Optionally, the melting rate of the electron gun is 16-60kg/h, and the melting power of the electron gun is 104-156 KW.
Optionally, the mold in the cooling system is a crucible, and the cooling time of the cooling system is more than or equal to 240 min.
Example (b):
the method comprises the following steps: taking 20kg Nb sawdust which is stored for about half a year and is not managed, taking out the Nb sawdust from oil stain, simply filtering and washing with clear water, and soaking in HNO3：H2In acid liquor with the volume ratio of O being 3: 1; the acid liquor exceeds the surface of the scraps by about 50mm, and the acid liquor is soaked for 25min and then is fed by clean waterRinsing was performed until the rinse water was neutral as measured by PH paper. Three Nb sawdust are randomly selected to analyze the content of the C element, and the content of the C element is lower than 200 ppm.
Step two: placing the cleaned Nb sawdust on a clean workbench to be naturally dried, paving the Nb sawdust on the workbench to be about 40mm in height, carrying out magnetic separation by using a magnet, and picking out the mixed steel wire brush residues and nuts.
Step three: and pressing the Nb scraps which are completely dried and subjected to magnetic separation by using a 500T oil press to obtain an electrode block, wherein the density of the electrode block is 5.2g/cm 3.
Assembling the pressed electrode blocks according to a mode of 1 multiplied by 6, welding in a vacuum welding box, evacuating the welding box before welding, performing side leakage when the vacuum degree is 1.22Pa/min, and controlling the air leakage rate to be 0.33 Pa/min. And welding the electrode blocks into an integral electrode for subsequent smelting.
Step four: and (3) filling the prepared electrode into a transverse feeding bin of the electron beam furnace, and evacuating the equipment. When the vacuum degree reaches 1.03Pa/min, the air leakage rate is 0.26 Pa/min. Smelting is started under the condition, the power at the stable stage is 125KW, the smelting speed reaches 42kg/h, and the steel is discharged after being cooled for 300 min.
Step five: sampling the head, the middle and the tail of the side wall of the cast ingot to analyze impurity elements.
The invention aims to protect a method for recovering and purifying Nb sawdust residues, which comprises the following steps: adding HNO3And H2Completely covering the mixed solution of O on the surface of the Nb sawdust, soaking for more than 20 minutes, and then cleaning for a certain time by using normal-temperature water; after the Nb sawdust is spread, magnetic substances in the Nb sawdust are screened out through magnetic separation; dividing the Nb sawdust into a plurality of equal parts and pressing the equal parts into a plurality of parts with the density of more than 4g/cm3The electrode blocks are welded into an electrode meeting the requirements of the electron beam furnace horizontal feeding through a vacuum argon arc welding box; and purifying the electrode by an electron beam furnace to obtain the Nb ingot. The process of treatment and recovery of the Nb sawdust residues is determined, and oil stains and cutting fluid on the surface of the Nb sawdust are removed by a surface treatment technology; the Nb filings mixed with a large amount of other metals are purified by an electron beam purification technology. Changes the situation that Nb sawdust generated in industrial production is treated as waste,the same-grade recovery of the Nb sawdust is realized, waste is changed into valuable, the Nb sawdust can be directly used as an intermediate alloy for product production after being processed, and precious metal resources are greatly saved.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (9)
1. A method for recovering and purifying residual Nb sawdust is characterized by comprising the following steps:
adding HNO3And H2Completely covering the mixed solution of O on the surface of the Nb sawdust, soaking for more than 20 minutes, and then cleaning for a certain time by using normal-temperature water;
after the Nb sawdust is flatly laid, magnetic substances in the Nb sawdust are screened out through magnetic separation;
dividing the Nb sawdust into a plurality of equal parts and pressing the equal parts into a plurality of parts with the density of more than 4g/cm3The electrode blocks are welded into an electrode meeting the requirements of the electron beam furnace horizontal feeding through a vacuum argon arc welding box;
and purifying the electrode by the electron beam furnace to obtain the Nb ingot.
2. The method of claim 1, wherein the welding of the plurality of electrode blocks into the electrode meeting the feeding requirement of the electron beam furnace through the vacuum argon arc welding box comprises the following steps:
before the electrode blocks are placed into the vacuum argon arc welding box for welding, the vacuum density of the vacuum argon arc welding box is kept to be less than or equal to 3Pa, the gas leakage rate of the vacuum argon arc welding box is less than or equal to 0.65Pa/min, and the welding current of the vacuum argon arc welding box is between 100A and 300A.
3. The method of claim 1, wherein said purifying said electrode through said electron beam furnace to obtain an Nb ingot comprises:
loading the electrode into a bin of the electron beam furnace in a cross-feed manner;
sealing the electron beam furnace and vacuumizing to ensure that the vacuum density is less than or equal to 3Pa, and adjusting the air leakage rate of the electron beam furnace to be less than or equal to 0.65 Pa/min;
smelting the electrode by using an electron gun of the electron beam furnace to obtain Nb liquid drops;
and injecting the Nb liquid drops into a mold in a cooling system of the electron beam furnace for cooling to obtain Nb ingots.
4. The method of claim 3,
the smelting speed of the electron gun is 16-60kg/h, and the smelting power of the electron gun is 104-156 KW.
5. The method of claim 3,
the cooling time of the cooling system is more than or equal to 240 min.
6. The method of claim 1,
the HNO3And H2In a mixed solution of O, HNO3：H2The volume ratio of O is 3: 1.
7. The method of claim 1,
before the magnetic separation screening is carried out, the method also comprises the following steps: and analyzing the content of the C element in the Nb sawdust.
8. The method of claim 1,
the time for cleaning the water with normal temperature is more than five minutes.
9. The method of claim 1,
the spreading thickness of the Nb sawdust is less than 50 mm.
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| CN202010145545.7A CN111621642A (en) | 2020-03-05 | 2020-03-05 | Method for recovering and purifying Nb sawdust residue |
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| CN202010145545.7A CN111621642A (en) | 2020-03-05 | 2020-03-05 | Method for recovering and purifying Nb sawdust residue |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4474604A (en) * | 1982-04-30 | 1984-10-02 | Hitachi Metals, Ltd. | Method of producing high-grade metal or alloy powder |
| US6007597A (en) * | 1997-02-28 | 1999-12-28 | Teledyne Industries, Inc. | Electron-beam melt refining of ferroniobium |
| CN101135010A (en) * | 2007-10-12 | 2008-03-05 | 西北有色金属研究院 | Method for recovering and reusing niobium and niobium alloy waste |
| CN101597693A (en) * | 2009-06-03 | 2009-12-09 | 宝鸡钛业股份有限公司 | A kind of preparation method of industrial pure zirconium ingot |
| CN101701298A (en) * | 2009-10-29 | 2010-05-05 | 国核宝钛锆业股份公司 | Manufacture method of nuclear grade zirconium-niobium alloy cast ingot |
| CN105950912A (en) * | 2016-06-30 | 2016-09-21 | 西部超导材料科技股份有限公司 | Preparation method for medical Zr-2.5 Nb alloy ingot |
| CN106435184A (en) * | 2015-08-21 | 2017-02-22 | 宁波创润新材料有限公司 | Technology for recovering metal chips |
-
2020
- 2020-03-05 CN CN202010145545.7A patent/CN111621642A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4474604A (en) * | 1982-04-30 | 1984-10-02 | Hitachi Metals, Ltd. | Method of producing high-grade metal or alloy powder |
| US6007597A (en) * | 1997-02-28 | 1999-12-28 | Teledyne Industries, Inc. | Electron-beam melt refining of ferroniobium |
| CN101135010A (en) * | 2007-10-12 | 2008-03-05 | 西北有色金属研究院 | Method for recovering and reusing niobium and niobium alloy waste |
| CN101597693A (en) * | 2009-06-03 | 2009-12-09 | 宝鸡钛业股份有限公司 | A kind of preparation method of industrial pure zirconium ingot |
| CN101701298A (en) * | 2009-10-29 | 2010-05-05 | 国核宝钛锆业股份公司 | Manufacture method of nuclear grade zirconium-niobium alloy cast ingot |
| CN106435184A (en) * | 2015-08-21 | 2017-02-22 | 宁波创润新材料有限公司 | Technology for recovering metal chips |
| CN105950912A (en) * | 2016-06-30 | 2016-09-21 | 西部超导材料科技股份有限公司 | Preparation method for medical Zr-2.5 Nb alloy ingot |
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Application publication date: 20200904 |