CN118374705B - Method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagation - Google Patents
Method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagationInfo
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Abstract
本发明涉及一种基于铝热自蔓延利用多场耦合制备CuAs合金的方法，属于冶金技术领域。本发明所述方法包括：(1)利用感应炉电热快速熔化金属纯铜得到铜熔体；(2)将Ca3(AsO4)2、Al粉混合物料利用机械搅拌和电磁搅拌产生的涡流引入铜熔体；(3)混合物料发生原位还原反应生成单质As和Al2O3‑CaO还原熔渣；(4)采用外加感应线圈进行保温熔炼；(5)Al2O3‑CaO还原熔渣采用溢流排渣法排出后经水淬直接制备铝酸钙水泥熟料，下层均质的CuAs合金熔体浇铸到水冷结晶器中进行快速冷却，该工艺采用还原和机械搅拌协同作用使As单质均匀弥散分布于Cu基体中，有效地解决了偏析问题，全程无废弃物排放，实现清洁制备CuAs合金。This invention relates to a method for preparing CuAs alloys based on aluminothermic self-propagation using multi-field coupling, belonging to the field of metallurgical technology. The method of this invention includes: (1) rapidly melting pure copper metal using an induction furnace to obtain copper melt; (2) introducing a mixture of Ca3 ( AsO4 ) 2 and Al powder into the copper melt using eddy currents generated by mechanical stirring and electromagnetic stirring; (3) the mixture undergoes an in-situ reduction reaction to generate elemental As and Al2O3 - CaO reduction slag; (4) using an external induction coil for heat preservation and smelting; (5) after the Al2O3 - CaO reduction slag is discharged by overflow slag discharge method, it is directly used to prepare calcium aluminate cement clinker by water quenching, and the lower homogeneous CuAs alloy melt is cast into a water-cooled crystallizer for rapid cooling. This process uses the synergistic effect of reduction and mechanical stirring to make elemental As uniformly dispersed in the Cu matrix, effectively solving the segregation problem, with no waste discharge throughout the process, and achieving clean preparation of CuAs alloy.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagation.
Background
CuAs the intermediate alloy is an alloy formed by adding As element into pure copper serving As a matrix, and is used for producing important additives of the As element in copper alloy and other special alloy materials. In the prior art, a pyrometallurgy process is mostly adopted for preparing alloy, and patent CN101423907a discloses a preparation method of tin-germanium-arsenic alloy, which comprises the steps of firstly reacting raw materials of arsenic, germanium and tin in a high-pressure reaction kettle to form intermediate alloy, then melting and refining the intermediate alloy with the rest tin and germanium, and casting to obtain the tin-germanium-arsenic alloy material. The method has high energy consumption and great pollution. Patent CN101748307a discloses a gold-arsenic alloy and a preparation method thereof, which comprises the steps of firstly weighing the raw materials according to the proportion, then placing the raw materials into an autoclave for reaction, controlling the pressure, the temperature and other changes in the autoclave to obtain an intermediate alloy ingot, then melting and refining the intermediate alloy ingot and the rest of gold together, and casting to obtain the gold-arsenic alloy material. The prior method for preparing CuAs intermediate alloy also has a null induction smelting method, namely, a vacuum induction furnace is adopted to smelt a high-purity electrolytic copper plate and nonmetallic As serving As raw materials at high temperature, and then the smelting is carried out by rapid solidification, so that the method increases the cost of the raw materials, and the method has the advantages of complex flow, high vacuum requirement, complex process and difficult temperature control.
In order to solve the technical problems of the existing copper-arsenic alloy synthesis process, application number 201910807554.5 provides a simple and low-cost method for synthesizing copper-arsenic alloy in situ from copper electrolyte, but the method cannot be used for preparing CuAs alloy on a large scale. Therefore, how to reduce the production cost of the prior production technology and prepare CuAS alloy with quality equivalent to and even better than commercial alloy performance so as to obtain good economic benefit is the research direction of CuAs alloy.
Disclosure of Invention
In order to solve the technical problems, the invention introduces vortex in the copper melt by adopting the synergistic effect of mechanical stirring and electromagnetic stirring, adds Ca 3(AsO4)2 powder and Al powder mixture into the melt, and carries out tempering of electromagnetic induction alloy melt under the protection of slag to ensure the effective separation of slag and gold, thus obtaining CuAs alloy and smelting slag of Al 2O3 -CaO.
A method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagation comprises the following steps:
(1) Heating to 1100-1300 ℃ by using an induction furnace to melt pure copper to obtain a copper melt;
(2) Forming a vortex within the copper melt;
(3) Uniformly mixing Al powder and Ca 3(AsO4)2, carrying the mixture into a copper melt through vortex, carrying out in-situ aluminothermic reduction reaction on the mixed material at the temperature of 1200-1400 ℃, and realizing dispersion addition of As in the copper melt under the action of multi-field coupling;
(4) Adopting an external induction coil to perform heat preservation smelting to obtain Al 2O3 -CaO reduction slag and CuAs alloy melt;
(5) Casting the CuAs alloy melt into a water-cooling crystallizer for rapid cooling to obtain CuAs alloy.
Further, the vortex in the step (2) is generated by using a straight blade type open turbine blade under the synergistic effect of mechanical stirring and electromagnetic stirring, and the stirring speed of the turbine blade is 200-300 rpm.
Further, the Al powder and the Ca 3(AsO4)2 in the step (3) are uniformly mixed according to the mol ratio of 10 (3-5).
Further, the addition amount of Ca 3(AsO4)2 in the step (3) is 1.1-1.3 times of the stoichiometric formula, the addition amount of As is controlled within the range of 20% -30%, the stoichiometric formula (1) is As follows, wherein x is 0.21-0.37 mol;
Cu+0.5xCa3(AsO4)2+5/3xAl＝[Cu-xAs]+5/6x(Al2O3·1.8CaO) (1)。
further, the step (3) is characterized in that Al powder and Ca 3(AsO4)2 are mixed on a ball mill for 30-60 min, and then pressed into a blank under 10-20 MPa.
Further, the smelting temperature in the step (4) is 1400-1600 ℃, the heat preservation time is 5-10 min, and the frequency of the externally-added induction coil is 3000-4500 Hz.
Further, the melting point of the Al 2O3 -CaO reduction slag in the step (4) is 1350-1550 ℃.
Further, the Al 2O3 -CaO reduction slag in the step (4) is directly subjected to water quenching by adopting an overflow slag discharge method to prepare the calcium aluminate cement clinker.
Compared with the prior art, the invention has the beneficial effects that:
(1) Compared with vacuum smelting, the method adopts Ca 3(AsO4)2 with lower price as the raw material, has low production cost, and does not need excessive vacuum degree when being prepared in a non-vacuum environment;
(2) Ca 3(AsO4)2 is used as a raw material, and slag formers such as CaO and the like are not needed to be added, so that CaO and Al 2O3 are directly generated in situ to carry out internal slag formation, and the energy loss is reduced.
(3) The generated CaO and Al 2O3 reduction slag are subjected to water quenching by adopting an overflow slag discharge method to prepare CA-50 brand, no waste is discharged in the whole process, and the CuAs alloy is prepared cleanly
(4) Compared with the traditional metallurgical method, the process adopts the synergistic effect of reduction and mechanical stirring to ensure that the As simple substances are uniformly dispersed and distributed in the Cu matrix, thereby effectively solving the segregation problem.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
Cu block, ca 3(AsO4)2 powder and Al powder were prepared according to the composition of CuAs gold ingot to be prepared, and Ca 3(AsO4)2 required for the reaction was placed in an oven and baked under 150 ℃ bars for 24 hours.
5Kg of Cu blocks are placed into an induction furnace, the temperature is raised to 1300 ℃ to enable the Cu blocks to be completely melted, the Cu blocks are in a melt state, and a mechanical stirring system is added. The stirring speed was set at 200rpm. 3317g of Ca 3(AsO4)2 powder and 750g of A1 powder were put into a mixing tank when the ingredients were mixed, mixed for 30 minutes in a ball mill, and the mixture was pressed into a green body under 10 MPa. Adding the blank into the melt in batches by vortex generated by mechanical stirring, generating an As simple substance in the melt by aluminothermic reduction reaction, uniformly dispersing the As simple substance in the melt by mechanical stirring and electromagnetic stirring to finally obtain a high-temperature melt composed of CuAs alloy melt and Al 2O3 -CaO reduction slag, smelting alloy slag by the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameter is 3000Hz, the smelting temperature is 1400 ℃, the smelting time is 5min, the upper layer forms the reduction slag, the lower layer forms the alloy melt, directly adopting an overflow slag discharging method to carry out water quenching to prepare CA-50 brand calcium aluminate cement clinker, casting the CuAs alloy melt into a water-cooling crystallizer to quickly solidify to obtain CuAs alloy cast ingots after slag removal, and the As content in the alloy is 19-21%.
Example 2
Cu block, ca 3(AsO4)2 powder and Al powder were prepared according to the composition of CuAs gold ingot to be prepared, and Ca 3(AsO4)2 required for the reaction was placed in an oven and baked under 150 ℃ bars for 24 hours.
5Kg of Cu blocks are placed into an induction furnace, the temperature is raised to 1300 ℃ to enable the Cu blocks to be completely melted, the Cu blocks are in a melt state, and a mechanical stirring system is added. The stirring speed was set at 200rpm. 3963g of Ca 3(AsO4)2 powder and 896g of A1 powder are put into a mixing tank when mixing ingredients, mixed for 30min on a ball mill, and the mixed materials are pressed into blanks under 13 MPa. Adding the blank into the melt in batches by vortex generated by mechanical stirring, generating an As simple substance in the melt by aluminothermic reduction reaction, uniformly dispersing the As simple substance in the melt by mechanical stirring and electromagnetic stirring to finally obtain a high-temperature melt composed of CuAs alloy melt and Al 2O3 -CaO reduction slag, smelting alloy slag by the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameter is 3500Hz, the smelting temperature is 1400 ℃, the smelting time is 8min, the upper layer forms the reduction slag, the lower layer forms the alloy melt, directly adopting an overflow slag discharging method to carry out water quenching to prepare CA-50 brand calcium aluminate cement clinker, casting the CuAs alloy melt into a water-cooling crystallizer to quickly solidify to obtain CuAs alloy cast ingots after slag removal, and the As content in the alloy is 21-24%.
Example 3
Cu block, ca 3(AsO4)2 powder and Al powder were prepared according to the composition of CuAs gold ingot to be prepared, and Ca 3(AsO4)2 required for the reaction was placed in an oven and baked under 150 ℃ bars for 24 hours.
5Kg of Cu blocks are placed into an induction furnace, the temperature is raised to 1300 ℃ to enable the Cu blocks to be completely melted, the Cu blocks are in a melt state, and a mechanical stirring system is added. The stirring speed was set at 200rpm. 4864g of Ca 3(AsO4)2 powder and 1000g of A1 powder are put into a mixing tank when mixing ingredients, mixed for 30min on a ball mill, and the mixture is pressed into a blank under 15 MPa. Adding the blank into the melt in batches by vortex generated by mechanical stirring, generating an As simple substance in the melt by aluminothermic reduction reaction, uniformly dispersing the As simple substance in the melt by mechanical stirring and electromagnetic stirring to finally obtain a high-temperature melt composed of CuAs alloy melt and Al 2O3 -CaO reduction slag, smelting the alloy slag of the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameter is 3800Hz, the smelting temperature is 1450 ℃, the smelting time is 10min, the upper layer forms the reduction slag, the lower layer forms the alloy melt, directly adopting an overflow slag discharging method to carry out water quenching to prepare CA-50 grade calcium aluminate cement clinker, casting the CuAs alloy melt into a water-cooling crystallizer to quickly solidify to obtain CuAs alloy cast ingots, and the As content in the alloy is 23-26%.
Example 4
Cu block, ca 3(AsO4)2 powder and Al powder were prepared according to the composition of CuAs gold ingot to be prepared, and Ca 3(AsO4)2 required for the reaction was placed in an oven and baked under 150 ℃ bars for 24 hours.
5Kg of Cu blocks are placed into an induction furnace, the temperature is raised to 1300 ℃ to enable the Cu blocks to be completely melted, the Cu blocks are in a melt state, and a mechanical stirring system is added. The stirring speed was set at 200rpm. 5675g of Ca 3(AsO4)2 powder and 1167g of A1 powder are put into a mixing tank when mixing ingredients, mixed for 30min on a ball mill, and the mixed materials are pressed into billets under 18 MPa. Adding the blank into the melt in batches by vortex generated by mechanical stirring, generating an As simple substance in the melt by aluminothermic reduction reaction, uniformly dispersing the As simple substance in the melt by mechanical stirring and electromagnetic stirring to finally obtain a high-temperature melt composed of CuAs alloy melt and Al 2O3 -CaO reduction slag, smelting alloy slag by the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameter is 4000Hz, the smelting temperature is 1450 ℃, the smelting time is 10min, the upper layer forms the reduction slag, the lower layer forms the alloy melt, directly adopting an overflow slag discharging method to carry out water quenching to prepare CA-50 brand calcium aluminate cement clinker, casting the CuAs alloy melt into a water-cooling crystallizer to quickly solidify to obtain CuAs alloy cast ingots after slag removal, and the As content in the alloy is 27-29%.
Example 5
Cu block, ca 3(AsO4)2 powder and Al powder were prepared according to the composition of CuAs gold ingot to be prepared, and Ca 3(AsO4)2 required for the reaction was placed in an oven and baked under 150 ℃ bars for 24 hours.
5Kg of Cu blocks are placed into an induction furnace, the temperature is raised to 1300 ℃ to enable the Cu blocks to be completely melted, the Cu blocks are in a melt state, and a mechanical stirring system is added. The stirring speed was set at 200rpm. 6823g of Ca 3(AsO4)2 powder and 1286g of A1 powder are put into a mixing tank when mixing ingredients, mixed for 30min on a ball mill, and the mixture is pressed into a blank under 20 MPa. Adding the blank into the melt in batches by vortex generated by mechanical stirring, generating an As simple substance in the melt by aluminothermic reduction reaction, uniformly dispersing the As simple substance in the melt by mechanical stirring and electromagnetic stirring to finally obtain a high-temperature melt composed of CuAs alloy melt and Al 2O3 -CaO reduction slag, smelting the alloy slag of the high-temperature melt under the action of an electromagnetic field, wherein the electromagnetic induction parameter is 4500Hz, the smelting temperature is 1500 ℃, the smelting time is 10min, the upper layer forms the reduction slag, the lower layer forms the alloy melt, directly adopting an overflow slag discharging method to carry out water quenching to prepare CA-50 grade calcium aluminate cement clinker, casting the CuAs alloy melt into a water-cooling crystallizer to quickly solidify to obtain CuAs alloy ingots, and the As content in the alloy is 29-32%.
Claims (8)
1. A method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagation is characterized by comprising the following steps:
(1) Heating to 1100-1300 ℃ by using an induction furnace to melt pure copper to obtain a copper melt;
(2) Forming a vortex within the copper melt;
(3) Uniformly mixing Al powder and Ca 3(AsO4)2, carrying the mixture into a copper melt through vortex, carrying out in-situ aluminothermic reduction reaction on the mixed material at the temperature of 1200-1400 ℃, and realizing dispersion addition of As in the copper melt under the action of multi-field coupling;
(4) Adopting an external induction coil to perform heat preservation smelting to obtain Al 2O3 -CaO reduction slag and CuAs alloy melt;
(5) Casting the CuAs alloy melt into a water-cooling crystallizer for rapid cooling to obtain CuAs alloy.
2. The method for preparing CuAs alloy by multi-field coupling based on self-propagating aluminothermic reaction according to claim 1, wherein the vortex in the step (2) is generated by using a straight blade open turbine blade under the synergistic effect of mechanical stirring and electromagnetic stirring, and the stirring speed of the turbine blade is 200-300 rpm.
3. The method for preparing CuAs alloy by using multi-field coupling based on self-propagating aluminothermic process as claimed in claim 1, wherein Al powder and Ca 3(AsO4)2 in step (3) are uniformly mixed according to a molar ratio of 10 (3-5).
4. The method for preparing CuAs alloy based on aluminothermic self-propagating multi-field coupling according to claim 1, wherein the addition amount of Ca 3(AsO4)2 in the step (3) is 1.1-1.3 times of stoichiometric formula (1), wherein x is 0.21-0.37 mol, and the addition amount of As is controlled within the range of 20% -30%;
Cu+0.5xCa3(AsO4)2+5/3xAl＝[Cu-xAs]+5/6x(Al2O3·1.8CaO) (1)。
5. The method for preparing CuAs alloy by multi-field coupling based on self-propagating aluminothermic reaction according to claim 1, wherein the uniform mixing in the step (3) is to mix Al powder and Ca 3(AsO4)2 on a ball mill for 30-60 min, and then press the mixture into a blank under 10-20 MPa.
6. The method for preparing CuAs alloy by utilizing multi-field coupling based on self-propagating aluminothermic reaction according to claim 1, wherein the smelting temperature in the step (4) is 1400-1600 ℃, the heat preservation time is 5-10 min, and the frequency of an externally added induction coil is 3000-4500 Hz.
7. The method for preparing CuAs alloy by utilizing multi-field coupling based on self-propagating aluminothermic process as set forth in claim 1, wherein the melting point of Al 2O3 -CaO reduction slag in the step (4) is 1350-1550 ℃.
8. The method for preparing CuAs alloy by utilizing multi-field coupling based on aluminothermic self-propagating according to claim 1, wherein the Al 2O3 -CaO reduction slag in step (4) is directly subjected to water quenching by adopting an overflow slag discharge method to prepare calcium aluminate cement clinker.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423907A (en) * | 2007-10-29 | 2009-05-06 | 北京有色金属与稀土应用研究所 | Sn-Ge-As alloy as well as preparation method and use thereof |
| CN115948667A (en) * | 2022-11-25 | 2023-04-11 | 国网辽宁省电力有限公司沈阳供电公司 | A kind of tungsten nanoparticle reinforced CuCr alloy and preparation method thereof |
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| CN101748307B (en) * | 2008-12-19 | 2012-07-25 | 北京有色金属与稀土应用研究所 | Gold-arsenic alloy material and preparation method thereof |
| CN107099718B (en) * | 2017-06-13 | 2018-08-28 | 东北大学 | The method for preparing ferro-tungsten with wash heat refining based on the reduction of aluminothermy self- propagating gradient |
| CN110453246B (en) * | 2019-08-28 | 2021-03-23 | 中南大学 | Method for in-situ synthesis of copper-arsenic alloy from copper electrolyte |
| CN117431418A (en) * | 2023-10-30 | 2024-01-23 | 中南大学 | A method for resource utilization of arsenic, antimony and alkali residues |
| CN117505788A (en) * | 2023-11-30 | 2024-02-06 | 国网辽宁省电力有限公司营口供电公司 | A method for preparing Invar steel ingots by aluminothermic self-propagation in-situ synthesis-slag refining |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423907A (en) * | 2007-10-29 | 2009-05-06 | 北京有色金属与稀土应用研究所 | Sn-Ge-As alloy as well as preparation method and use thereof |
| CN115948667A (en) * | 2022-11-25 | 2023-04-11 | 国网辽宁省电力有限公司沈阳供电公司 | A kind of tungsten nanoparticle reinforced CuCr alloy and preparation method thereof |
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