CN111500829B - Method for quenching and recycling waste hard alloy - Google Patents
Method for quenching and recycling waste hard alloy Download PDFInfo
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- CN111500829B CN111500829B CN202010342265.5A CN202010342265A CN111500829B CN 111500829 B CN111500829 B CN 111500829B CN 202010342265 A CN202010342265 A CN 202010342265A CN 111500829 B CN111500829 B CN 111500829B
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- C21D1/18—Hardening; Quenching with or without subsequent tempering
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Abstract
The invention belongs to the field of waste hard alloy recovery, and relates to a method for quenching and recovering waste hard alloy. The method for recycling the waste hard alloy comprises the steps of sequentially quenching, crushing and electro-dissolving the clean and dry waste hard alloy, wherein the quenching is carried out in a medium-frequency furnace. The method provided by the invention is adopted to quench and recover the waste hard alloy, has the advantages of high heating speed, high efficiency, low energy consumption and good quenching effect, is beneficial to crushing the waste hard alloy, has less burning loss of the hard alloy in the quenching process, and has higher purity and yield of the obtained hard alloy.
Description
Technical Field
The invention belongs to the field of waste hard alloy recovery, and particularly relates to a method for quenching and recovering waste hard alloy.
Background
Cemented carbide is an alloy material made from a hard compound of refractory metals and a binder metal by a powder metallurgy process. At present, the waste hard alloy is generally recycled by adopting a process comprising quenching, crushing and electro-dissolving in sequence. In this case, quenching is generally performed in an electric resistance furnace. However, the method for recycling the waste hard alloy has lower purity and yield of the obtained hard alloy.
Disclosure of Invention
The invention aims to overcome the defect that the purity and yield of the obtained hard alloy are lower when the existing method is used for recovering the waste hard alloy, and provides a novel method for quenching and recovering the waste hard alloy.
After intensive research, the inventors of the present invention found that when the existing method including quenching, crushing and electro-dissolution is used to recover the waste hard alloy, the quenching process has a very important influence on the purity and yield of the recovered hard alloy. The traditional quenching mode is heating quenching by a resistance furnace. However, the resistance furnace heats the materials in the furnace by heating the electric heating elements in the furnace by using current, the surface of the object is heated by heat radiation, the heating speed is low, the efficiency is low, the energy loss is large, the heating uniformity is poor, the quenching effect of the waste hard alloy is poor, the burning loss of alloy elements is large, and the purity and the yield of the hard alloy can be greatly reduced. The medium frequency furnace mainly comprises a power supply, an induction coil and a crucible built by refractory materials in the induction coil, when the medium frequency furnace is adopted to replace a resistance furnace for quenching, waste hard alloy is placed in the crucible, when the induction coil is connected with an alternating current power supply, an alternating magnetic field is generated in the induction coil, magnetic lines of force cut the hard alloy material in the crucible, induced electromotive force is generated in furnace charge, and induced current is generated at the same time to realize heating of the furnace charge, the heating and quenching mode has the advantages of high heating speed, high efficiency and low energy consumption, when the medium frequency furnace is adopted to heat the waste hard alloy, high-density magnetic lines of force are generated in the induction coil, the waste hard alloy placed in the induction coil is cut, and great eddy current is generated in the hard alloy, so that the hard alloy is rapidly and uniformly heated from inside to outside, the quenching effect after heating is good, and the crushing of the waste hard alloy is facilitated, the burning loss of alloy elements is less, and the purity and the yield of the hard alloy are improved. Based on this, the present invention has been completed.
Specifically, the invention provides a method for quenching waste hard alloy, wherein the method comprises the step of quenching the waste hard alloy in a medium-frequency furnace.
Further, the waste hard alloy is cobalt-tungsten alloy and/or tungsten-copper alloy.
Further, the quenching temperature is 1300-1400 ℃, and the quenching time is 1-2 hours.
Further, the quenching process comprises the steps of putting the waste hard alloy into a graphite crucible of an intermediate frequency furnace, adjusting the initial power of the intermediate frequency furnace to 3-4kw, starting heating, then increasing the power by 2kw every 5-15 minutes, simultaneously monitoring the temperature of the surface of the waste hard alloy, keeping the temperature for 1-2 hours after the temperature reaches the quenching temperature, and then cooling to the room temperature at the rate of 400 plus 500 ℃/minute.
The invention also provides a method for recycling the waste hard alloy, wherein the method comprises the steps of sequentially quenching, crushing and electro-dissolving the clean and dry waste hard alloy, and the quenching is carried out by adopting the method.
Further, the crushing conditions are such that the particle size of the crushed product is 20-40 mm.
Further, the waste hard alloy is cobalt-tungsten alloy and/or tungsten-copper alloy.
Further, the electrolytic solution is prepared by loading the crushed product into an anode basket as an anode, electrolyzing by using a titanium material as a cathode, crushing and cleaning the anode in sequence to remove impurities to obtain tungsten carbide after the electrolysis is completed, and purifying the electrolyte to obtain the metal cobalt.
Further, the anode crushing condition is that the particle size of the obtained crushed product is 5-10 mm.
Further, the cleaning agent used for cleaning and impurity removing is at least one selected from dilute nitric acid, dilute hydrochloric acid and dilute sodium hydroxide solution.
Further, the purification step comprises removing iron from the electrolyte, extracting and removing impurities from the iron-removed feed liquid by using P204, and back-extracting and removing impurities from the raffinate by using P507, wherein the back-extract is pure cobalt chloride or cobalt sulfate solution.
The method provided by the invention is adopted to quench and recover the waste hard alloy, has high efficiency, low energy consumption and good quenching effect, is beneficial to crushing the waste hard alloy, has less burning loss of hard alloy elements in the quenching process, and has higher purity and yield of the obtained hard alloy.
Drawings
Fig. 1 is a specific flow diagram of the quenching method of waste hard alloy provided by the invention.
Detailed Description
The method provided by the invention is particularly suitable for quenching and recycling the hard alloy such as cobalt-tungsten alloy, tungsten-copper alloy and the like. The cobalt-tungsten alloy comprises a high cobalt-tungsten alloy and a low cobalt-tungsten alloy. The cobalt content in the high cobalt tungsten alloy is 10-20 wt%, and the tungsten content is 80-90 wt%. The content of cobalt in the low-cobalt tungsten alloy is 5-9 wt%, and the content of tungsten is 91-95 wt%.
In the invention, the waste hard alloy to be quenched can be bars, rollers, spherical teeth and the like. When quenching, the alloy size is generally not more than 1/3 of the inner diameter of the crucible of the intermediate frequency furnace, so that not only the quenching efficiency can be improved, but also the impact on the furnace wall and the furnace bottom in the feeding process can be prevented.
The intermediate frequency furnace is a power supply device for converting power frequency 50HZ alternating current into intermediate frequency (300-1000 HZ). As shown in figure 1, the intermediate frequency furnace comprises a heating furnace and a material frame, wherein a crucible is arranged in the heating furnace, and the material frame is arranged in a water pool. When the waste hard alloy is quenched by adopting an intermediate frequency furnace, the waste hard alloy is placed in a crucible in a heating furnace, the power is adjusted to 3-4kw to start heating, then the power is increased by 2kw every 5-15 minutes, meanwhile, the temperature of the surface of the waste hard alloy is monitored, when the temperature reaches the quenching temperature (1300 plus 1400 ℃) and is kept for 1-2 hours, and then the waste hard alloy is cooled to the room temperature at the speed of 400 plus 500 ℃/minute. The specific cooling process is that a speed reducer is adopted to pour the waste hard alloy to be cooled in the crucible into a material frame in a water tank for quenching, after the waste hard alloy is cooled to normal temperature, a travelling crane is used for lifting the quenched material frame out of the water, and the waste hard alloy is easy to crush after being quenched, so that the waste hard alloy is crushed to the granularity of 20-40 mm.
The method for recycling the waste hard alloy comprises the steps of sequentially quenching, crushing and electro-dissolving the clean and dry waste hard alloy, wherein the quenching is carried out by adopting the method.
The conditions for the crushing are not particularly limited in the present invention, and the particle size of the obtained crushed product is preferably 20 to 40mm, which is more advantageous for the subsequent anode electro-dissolution purification. Further, the crushing may be performed by, for example, crushing, impact crushing, shattering, grinding, or the like.
In the invention, the function of the electro-dissolution is to purify and remove impurities from the quenched waste hard alloy. Taking waste cobalt-tungsten alloy as an example, the electrolytic solution can be specifically prepared by loading the crushed product into an anode basket as an anode, electrolyzing by taking a titanium material as a cathode, crushing and cleaning the anode in sequence after the electrolysis is finished to remove impurities to obtain tungsten carbide, and purifying the electrolyte to obtain the metal cobalt. After electrolysis, metal cobalt and most impurities in the waste cobalt-tungsten alloy enter the electrolyte, tungsten carbide is left in the anode basket, the tungsten carbide with high purity can be obtained after crushing, cleaning and impurity removal of the residual anode, and the metal cobalt can be obtained after further purifying and purifying the electrolyte. The cleaning agent used for cleaning and impurity removing can be at least one selected from dilute nitric acid, dilute hydrochloric acid and dilute sodium hydroxide solution. The concentration of the above cleaning agent is generally 0.5 to 1 mol/L. The step of purifying may specifically include removing iron from the electrolyte (the iron removal method may be, for example, a sodium-yellow iron-vanadium method), extracting the obtained iron-removed feed liquid with P204 to remove impurities of calcium, copper, manganese, and zinc, back-extracting the obtained raffinate with P507 to remove impurities of nickel and magnesium, and obtaining the back-extract, which is pure cobalt chloride or cobalt sulfate.
According to a specific embodiment of the present invention, the electrolyte used for the electrolysis comprises the following components in percentage by weight: cobalt: 35-40g/L, nickel: 1000-1500mg/L, iron: 5-20mg/L, copper: 10-15mg/L, calcium: 0.5-1mg/L, magnesium: 0.4-0.6mg/L, manganese: 0.1-0.3mg/L, zinc: 0.4-0.8mg/L, chromium: 0.1-0.2mg/L, cadmium: 0.2-0.5 mg/L. The conditions for the electrolysis generally include a temperature of 30-60 ℃ and a current density of 200-400A/m2The electrolysis time is 20-30 hours.
The present invention will be described in detail below by way of examples.
In the following examples, the purity of the waste hard alloy was measured by fluorescence spectroscopy, and the yield was measured by atomic absorption spectroscopy.
Example 1
(1) Quenching and crushing:
4.5 kg of waste hard alloy (cobalt-tungsten alloy) bar materials are placed in a graphite crucible of an intermediate frequency furnace, the initial power of the intermediate frequency furnace is adjusted to 3.5kw, heating is started, the power is increased by 2kw every 10 minutes, the temperature of the alloy is rapidly increased from inside to outside, and the alloy turns red. And when the power rises by 2kw, measuring the temperature of the surface of the hard alloy by adopting an infrared thermometer. The whole temperature rise process is only 50 minutes, the temperature reaches about 1300 ℃ required by the quenching process, and the temperature is kept for 1 hour at the quenching temperature. For a common resistance furnace, the time of the whole temperature rise process is 3 hours, and after the temperature reaches the process requirement, the heat is preserved for 1 hour. Therefore, compared with a resistance furnace, the heating efficiency of the intermediate frequency furnace is improved remarkably. The cobalt content, density, hardness and bending strength results of the waste hard alloy before and after quenching are shown in table 1.
Starting a speed reducer to dump the furnace body, pouring the hard alloy at high temperature into a material frame in a water tank, and carrying out high-temperature quenching operation at the speed of 400-. After the waste hard alloy is cooled to normal temperature, the quenched material frame is lifted out of the water by a travelling crane, and the waste hard alloy is easy to break after being quenched. Then putting the hard alloy into a crusher for crushing, and crushing the hard alloy until the grain diameter is 20-40 mm.
(2) And (3) electro-dissolving:
putting the crushed hard alloy into anode blue as an anode, taking a titanium material as a cathode, and taking dilute hydrochloric acid as electrolyte for electrolysis, wherein the electrolysis temperature is 45 ℃, and the current density is 300A/m2The electrolysis time was 24 hours. The electrolyte comprises the following components:
after the electrolysis is finished, crushing the anode to the particle size of 5-10mm, and then cleaning and removing impurities by using dilute nitric acid with the concentration of 0.6mol/L to obtain the tungsten carbide. Removing iron from the electrolyte by using a crude cobalt solution, removing impurities such as calcium, copper, manganese and zinc from the iron-removed feed liquid by using P204, separating the impurities such as nickel and magnesium from the extract liquid by using P507 cobalt back extraction, and obtaining a back extraction product which is a pure cobalt chloride solution. The purity of tungsten carbide and cobalt chloride and the yield of tungsten and cobalt are shown in table 2.
Comparative example 1
The waste hard alloy was recovered according to the method of example 1, except that the quenching was performed using a resistance furnace instead of a medium frequency furnace, and the results of cobalt content, density, hardness and bending strength after quenching of the waste hard alloy are shown in table 1. The purity of the tungsten carbide and cobalt chloride and the yield of tungsten and cobalt are shown in table 2.
TABLE 1
TABLE 2
As can be seen from the results in tables 1 and 2, when the method of the present invention is used to quench the used cemented carbide, the burning loss of the cemented carbide is small, and the bending strength is significantly reduced. In addition, the method provided by the invention can be used for recovering the waste hard alloy, so that the purity and the yield of the obtained hard alloy can be improved.
Example 2
(1) Quenching and crushing:
6.2 kg of waste hard alloy (cobalt-tungsten alloy) bar materials are placed into a graphite crucible of an intermediate frequency furnace, the initial power of the intermediate frequency furnace is adjusted to 3.5kw, heating and quenching are started, the power is increased by 2kw every 8 minutes, the temperature of the alloy is rapidly increased from inside to outside, and the alloy turns red. When the power rises by 2kw, the temperature of the surface of the hard alloy is measured by an infrared thermometer, and the temperature rises rapidly. The whole temperature rise process is only 40 minutes, the temperature reaches about 1400 ℃ required by the process, and the quenching temperature is kept for 2 hours. For a common resistance furnace, the time of the whole temperature rise process is 3 hours, and after the temperature reaches the process requirement, the heat is preserved for 2 hours. Therefore, compared with a resistance furnace, the heating efficiency of the intermediate frequency furnace is improved remarkably. The cobalt content, density, hardness and bending strength results of the waste cemented carbide before and after quenching are shown in table 3.
Starting a speed reducer to dump the furnace body, pouring the hard alloy at high temperature into a material frame in a water tank, and carrying out high-temperature quenching operation at the speed of 400-. After the waste hard alloy is cooled to normal temperature, the quenched material frame is lifted out of the water by a travelling crane, and the waste hard alloy is easy to break after being quenched. Then putting the hard alloy into a crusher for crushing, and crushing the hard alloy until the grain diameter is 20-40 mm.
(2) And (3) electro-dissolving:
charging crushed hard alloy into the anodeThe electrode basket is used as an anode, the titanium material is used as a cathode, the dilute hydrochloric acid is used as electrolyte for electrolysis, the electrolysis temperature is 45 ℃, and the current density is 300A/m2The electrolysis time was 20 hours. The electrolyte comprises the following components:
after the electrolysis is finished, crushing the anode to the particle size of 5-10mm, and then cleaning and removing impurities by adopting a dilute sodium hydroxide solution with the concentration of 0.5mol/L to obtain the tungsten carbide. Removing iron from the electrolyte by using a crude cobalt solution, removing impurities such as calcium, copper, manganese and zinc from the iron-removed feed liquid by using P204, separating the impurities such as nickel and magnesium from the extract liquid by using P507 cobalt back extraction, and obtaining a back extraction product which is the pure cobalt sulfate solution. The purity of tungsten carbide and cobalt sulfate and the yield of tungsten and cobalt are shown in table 4.
Comparative example 2
The waste hard alloy was recovered according to the method of example 2, except that the quenching was performed using a resistance furnace instead of a medium frequency furnace, and the results of cobalt content, density, hardness and bending strength after quenching of the waste hard alloy are shown in table 3. The purity of the tungsten carbide and cobalt chloride and the yield of tungsten and cobalt are shown in table 4.
TABLE 3
TABLE 4
As can be seen from the results in tables 3 and 4, when the method of the present invention is used to quench the used cemented carbide, the burning loss of the cemented carbide is small and the bending strength is significantly reduced. In addition, the method provided by the invention can be used for recovering the waste hard alloy, so that the purity and the yield of the obtained hard alloy can be improved.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (7)
1. The method for recycling the waste hard alloy is characterized by comprising the steps of sequentially quenching, crushing and electro-dissolving clean and dry waste hard alloy, wherein the quenching comprises the steps of putting the waste hard alloy into an intermediate frequency furnace for quenching, the frequency of the intermediate frequency furnace is 300-.
2. The method for recycling the waste hard alloy as claimed in claim 1, wherein the quenching is carried out by putting the waste hard alloy into a crucible of an intermediate frequency furnace, adjusting the initial power of the intermediate frequency furnace to 3-4kw for starting heating, and then increasing the power by 2kw every 5-15 minutes while monitoring the temperature of the surface of the waste hard alloy.
3. The method for recycling waste hard alloy according to claim 1, characterized in that the crushing conditions are such that the particle size of the obtained crushed product is 20-40 mm.
4. The method for recycling waste hard alloy according to any one of claims 1 to 3, wherein the waste hard alloy is cobalt tungsten alloy and/or tungsten copper alloy.
5. The method for recycling the waste hard alloy according to the claim 1 or 3, characterized in that the waste hard alloy is cobalt-tungsten alloy, the electrolysis is carried out by putting the crushed product into an anode basket as an anode, and taking titanium as a cathode for electrolysis, after the electrolysis is completed, the anode is crushed, cleaned and purified in sequence to obtain tungsten carbide, and the electrolyte is purified to obtain metal cobalt.
6. The method for recycling waste hard alloy according to claim 5, characterized in that the anode crushing conditions are such that the particle size of the crushed product is 5-10 mm; the cleaning agent adopted for cleaning and impurity removal is at least one selected from dilute nitric acid, dilute hydrochloric acid and dilute sodium hydroxide solution.
7. The method for recycling waste hard alloy according to claim 5, wherein the step of purifying comprises removing iron from the electrolyte, the feed liquid after removing iron is subjected to extraction and impurity removal by using P204, the raffinate is subjected to back extraction and impurity removal by using P507, and the back extract is pure cobalt chloride or cobalt sulfate solution.
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Citations (4)
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| US4234333A (en) * | 1979-04-25 | 1980-11-18 | Fansteel, Inc. | Process for recovering metal carbide powder from cemented carbides |
| JP2000072430A (en) * | 1998-08-28 | 2000-03-07 | Wada Kogyo Kk | Repowdering technique for spent sintered hard alloy part by tin impregnation method |
| CN101054640A (en) * | 2007-05-21 | 2007-10-17 | 陈兆盈 | Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC |
| CN103409634A (en) * | 2013-08-15 | 2013-11-27 | 自贡三盛硬质合金有限公司 | Recovery method for waste hard alloy and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1100147A (en) * | 1994-08-15 | 1995-03-15 | 自贡长域工具公司 | Method for treatment of waste low-cobalt alloy by electro-dissolving and crushing-magnetic selection |
| CN1147988A (en) * | 1995-10-16 | 1997-04-23 | 崔士杰 | Two-in-one working art for medium frequency welding and quenching coal cutter teeth |
| CN108467041A (en) * | 2018-04-26 | 2018-08-31 | 南昌大学 | A method of the recovered WC from useless coated carbides |
| CN108977664B (en) * | 2018-07-24 | 2019-10-29 | 中南大学 | The method for recycling tungsten carbide and cobalt in scrap hard alloy |
| CN109022769B (en) * | 2018-08-27 | 2020-04-03 | 河北罗奇新材料科技有限公司 | Process for recovering tungsten and cobalt in tungsten-cobalt alloy waste |
| CN108910966B (en) * | 2018-09-21 | 2020-06-09 | 湖南金雕能源科技有限公司 | Method for extracting tungsten carbide and cobalt from waste hard alloy |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234333A (en) * | 1979-04-25 | 1980-11-18 | Fansteel, Inc. | Process for recovering metal carbide powder from cemented carbides |
| JP2000072430A (en) * | 1998-08-28 | 2000-03-07 | Wada Kogyo Kk | Repowdering technique for spent sintered hard alloy part by tin impregnation method |
| CN101054640A (en) * | 2007-05-21 | 2007-10-17 | 陈兆盈 | Vacuum high temperature treatment method for reducing oxygen content of electric dissolving regeneration WC |
| CN103409634A (en) * | 2013-08-15 | 2013-11-27 | 自贡三盛硬质合金有限公司 | Recovery method for waste hard alloy and application |
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