CN111187917B - Removing agent and removing method for low-content impurity element tin in copper melt - Google Patents
Removing agent and removing method for low-content impurity element tin in copper melt Download PDFInfo
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- CN111187917B CN111187917B CN202010118497.2A CN202010118497A CN111187917B CN 111187917 B CN111187917 B CN 111187917B CN 202010118497 A CN202010118497 A CN 202010118497A CN 111187917 B CN111187917 B CN 111187917B
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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
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
- C22B9/103—Methods of introduction of solid or liquid refining or fluxing agents
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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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/006—Pyrometallurgy working up of molten copper, e.g. refining
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
The invention provides a remover and a removing method for low-content impurity element tin in a copper melt. The remover comprises a refining agent and a deslagging agent. The copper material suitable for the invention refers to copper and copper alloy materials containing tin as an impurity element, wherein the tin content is 0.0003-3% by weight. According to the method, the removing agent is added into the copper melt, so that the impurity element tin in the copper melt can be effectively removed, the effect of purifying the copper melt is achieved, and the content of tin in the copper material after the impurity element tin is removed by the method is less than 10 ppm.
Description
Technical Field
The invention relates to a method for removing low-melting-point impurity elements in non-ferrous metal materials, in particular to a remover and a removing method for low-melting-point impurity element tin in copper and copper alloy.
Background
Copper has good electric and heat conducting properties and is widely used for electric and heat conducting devices, such as integrated circuit boards, computer mainboards, electric conducting contacts, evaporating pipes, condensing pipes and the like used in the air conditioning and refrigeration industries. The trace impurity element tin in copper belongs to solid solution impurities, and can reduce the electric and heat conducting performance of copper. The first and second oxygen-free copper generally require less than 20ppm tin. In the actual smelting process of copper, the content of tin often exceeds the standard due to the use of various scrap copper and scrap returns. The removal effect of various refining agents used in the current market on tin element is not good. Tin has a melting point of 231.9 ℃ which is much lower than that of copper, and is an impurity element having a low melting point. The invention provides a remover and a removing method for impurity element tin in a copper melt, aiming at the technical problem that the impurity element tin in the copper melt is difficult to remove.
Disclosure of Invention
The invention provides a remover for removing low-content impurity element tin in a copper melt and a method for removing the low-content impurity element tin in the copper melt, aiming at solving the defects and the hazards caused by the low-melting-point impurity element tin in copper and copper alloy materials in the prior art.
The copper material suitable for the invention refers to copper and copper alloy materials containing low-melting-point impurity element tin, wherein the content of the impurity element tin is 0.0003-3% by weight.
In order to achieve one of the above objects, the technical solution of the present invention is as follows:
a remover for removing low-content impurity element tin from a copper melt comprises a refining agent and a deslagging agent.
A refining agent for removing impurity element tin in the copper melt,
the refining agent is intermediate alloy of rare earth elements of yttrium, praseodymium, neodymium, europium and copper, and is calculated by weight percentage,
1-20% of rare earth yttrium,
1 to 5 percent of praseodymium,
3-18% of neodymium,
2 to 15 percent of europium,
The balance being copper.
Preferably, the refining agent has a particle size of 50 to 200 mesh.
A slag removing agent for removing impurity element tin in the copper melt,
the slag remover consists of sodium carbonate, sodium borate, sodium chloride and calcium fluoride, and is calculated by weight percentage,
20-60% of sodium carbonate,
10-50% of sodium borate,
10-20% of sodium chloride,
5 to 20 percent of calcium fluoride,
The balance of inevitable impurities and the content of the impurities is 0 to 1 percent.
Preferably, the particle size of the deslagging agent is 150-400 meshes.
In order to achieve the second object of the invention, the technical scheme of the invention is as follows:
a method for removing low-content impurity element tin in a copper melt comprises the following steps,
putting the copper material containing impurity element tin into a smelting furnace, controlling the temperature at 1150-1250 ℃ to completely melt the copper material into copper liquid, covering graphite powder covering agent with the thickness of 10-30 cm on the surface of the copper liquid in the melting process to pre-deoxidize and isolate air, obtaining copper melt after 30-60 minutes,
secondly, the refining agent of claim 1 is wrapped by copper foil and then pressed into the copper melt by a graphite bell jar for refining for 20 to 60 minutes,
and the content of the additive is calculated by weight percentage,
when the content of tin in the copper melt is 0.0003-0.03% and not including 0.03%, the refining agent is added in an amount of 0.01-0.1% and not including 0.1% of the copper melt,
when the content of tin in the copper melt is 0.03-1% and not 1%, the refining agent is added in an amount of 0.1-3% and not 3% of the copper melt,
when the tin content in the copper melt is 1-3%, the adding amount of the refining agent is 3-8% of the copper melt;
thirdly, adding the slag removing agent in the claim 2 into the copper melt and stirring for 15 to 30 minutes, wherein the adding amount of the slag removing agent is 3 to 8 grams in each 100 grams of the copper melt according to the weight percentage,
then standing for 20-40 minutes, and removing dross on the surface of the copper melt by using a dross scooping spoon;
fourthly, pouring the copper melt after deslagging into a preheated mould to obtain the copper material with low melting point impurity element tin removed.
The content of tin element in the copper material after removing the impurity element tin by the method is less than 10 ppm.
Advantageous effects
The copper material suitable for the invention refers to copper and copper alloy materials containing tin as an impurity element, wherein the tin content is 0.0003-3% by weight. According to the method, the removing agent is added into the copper melt, so that the impurity element tin in the copper melt can be effectively removed, the effect of purifying the copper melt is achieved, and the content of tin in the copper material after the impurity element tin is removed by the method is less than 10 ppm.
Drawings
Fig. 1 is a photograph of the metallographic structure of a copper material to which a refining agent is added according to the present invention.
Fig. 2 is a photograph of the metallographic structure of the copper material to which the refining agent and the slag removing agent have been added.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments, not all embodiments, of the present patent. All other embodiments, which can be derived by a person skilled in the art from the embodiments given in this patent without making any creative effort, shall fall within the protection scope of the present invention.
Example 10.005% tin copper
The method for removing impurity element tin in the copper melt comprises the following specific steps: putting 8.96 kilograms of copper material containing 0.005 percent of tin into a smelting furnace, adopting a graphite orange pan, controlling the temperature to be 1158 ℃, and completely melting the copper material into copper liquid; covering a layer of graphite powder covering agent on the surface of the molten copper, wherein the thickness of the covering agent is 18 cm; 3.64 g of refining agent is added into the smelted copper melt, wherein, in percentage by weight, 78% of copper, 8% of rare earth yttrium, 3% of praseodymium, 5% of neodymium and 6% of europium are added. Wrapping the refining agent with copper foil, pressing in with a graphite bell jar, and refining for 38 minutes; adding 268.81 g of deslagging agent into the refined copper liquid, wherein the weight percentage of sodium carbonate is 25%, the weight percentage of sodium borate is 40%, the weight percentage of sodium chloride is 18%, and the weight percentage of calcium fluoride is 17%, thoroughly stirring the copper liquid for 26 minutes, then standing the copper liquid for 33 minutes, removing scum on the surface of the copper melt by using a slag spoon, pouring the copper liquid into a preheated mold to obtain the copper material with the impurity element tin removed, and detecting that the content of the impurity element tin in the copper material is only 4 ppm.
Example 20.016% tin copper
The method for removing impurity element tin in the copper melt comprises the following specific steps: 9.21 kg of copper material containing 0.016 percent of tin is put into a smelting furnace, a graphite orange pan is adopted, the temperature is controlled at 1182 ℃, and the copper material is completely melted into copper liquid; covering a layer of graphite powder covering agent on the surface of the molten copper, wherein the thickness of the covering agent is 21 cm; 7.41 g of refining agent is added into the smelted copper melt, wherein, according to the weight percentage, 75 percent of copper, 12 percent of rare earth yttrium, 2 percent of praseodymium, 7 percent of neodymium and 4 percent of europium are added. Wrapping the refining agent with copper foil, pressing in with a graphite bell jar, and refining for 42 minutes; 198.62 g of deslagging agent is added into the refined copper liquid, wherein, by weight percentage, 40% of sodium carbonate, 35% of sodium borate, 12% of sodium chloride and 13% of calcium fluoride are added into the copper liquid, the copper liquid is thoroughly stirred for 22 minutes, then the copper liquid is kept still for 27 minutes, scum on the surface of the copper melt is removed by a slag spoon, and then the copper liquid is poured into a preheated mould to obtain the copper material with the impurity element tin removed, and the content of the impurity element tin in the copper material is only 6ppm through detection.
Example 31.12% tin copper
The method for removing impurity element tin in the copper melt comprises the following specific steps: 8.79 kg of copper material containing 1.12 percent of tin is put into a smelting furnace, a graphite orange pan is adopted, the temperature is controlled at 1240 ℃, and the copper material is completely melted into copper liquid; covering a layer of graphite powder covering agent on the surface of the molten copper, wherein the thickness of the covering agent is 25 cm; 281.26 g of refining agent is added into the smelted copper melt, wherein, the weight percentage is calculated by 72 percent of copper, 10 percent of rare earth yttrium, 4 percent of praseodymium, 4 percent of neodymium and 10 percent of europium. Wrapping the refining agent with copper foil, pressing in with a graphite bell jar, and refining for 31 minutes; 307.65 g of deslagging agent is added into the refined copper liquid, wherein, the weight percentage of sodium carbonate is 32%, the weight percentage of sodium borate is 36%, the weight percentage of sodium chloride is 14%, and the weight percentage of calcium fluoride is 18%, the copper liquid is thoroughly stirred for 19 minutes, then the copper liquid is kept still for 30 minutes, after scum on the surface of the copper melt is removed by a scum spoon, the copper liquid is poured into a preheated mould, and the copper material with the impurity element tin removed is obtained, and the detected content of the impurity element tin in the copper material is only 5 ppm.
Example 42.33% tin copper
The method for removing impurity element tin in the copper melt comprises the following specific steps: 9.83 kilograms of copper materials containing 2.33 percent of tin are put into a smelting furnace, a graphite orange pan is adopted, the temperature is controlled at 1225 ℃, and the copper materials are completely melted into copper liquid; covering a layer of graphite powder covering agent on the surface of the molten copper, wherein the thickness of the covering agent is 30 cm; 681.13 g of refining agent is added into the smelted copper melt, wherein, the weight percentage is calculated, the copper is 70 percent, the rare earth yttrium is 12 percent, the praseodymium is 5 percent, the neodymium is 5 percent, and the europium is 8 percent. Wrapping the refining agent with copper foil, pressing in with a graphite bell jar, and refining for 27 minutes; 275.24 g of deslagging agent is added into the refined copper liquid, wherein the sodium carbonate is 51 percent, the sodium borate is 23 percent, the sodium chloride is 18 percent and the calcium fluoride is 8 percent by weight percent, the copper liquid is thoroughly stirred for 16 minutes, then the copper liquid is kept still for 36 minutes, scum on the surface of the copper melt is removed by a slag spoon, the copper liquid is poured into a preheated die, and the copper material with the impurity element tin removed is obtained, and the content of the impurity element tin in the copper material is detected to be 3 ppm.
The content of tin element in the copper material after removing the impurity element tin by the method is less than 10ppm, compared with the technical index of 20ppm of tin element in the oxygen-free copper I and II in the prior art, the content of tin element in the copper material is improved by 1 time, and the content of tin element in the copper material can be reduced to about 5ppm at least in the preferred embodiments 1-4 in the specific implementation mode of the invention, which shows that the refining agent, the deslagging agent and the removal method can effectively remove the impurity element tin in the copper melt, and the removal effect is obvious and is far higher than the standard requirement of tin content in the oxygen-free copper I and II.
Theoretically, yttrium, praseodymium, neodymium and europium elements have very low Gibbs free energy change values and very high chemical reaction equilibrium constants, and tests of the invention also prove that the yttrium, praseodymium, neodymium and europium elements can react with tin completely even if the content of tin is low, the yttrium, praseodymium, neodymium and europium elements in the refining agent can capture impurity element tin in copper melt and react to generate complex compound particles of the rare earth elements and tin, and the impurity element tin dispersed and dissolved in copper can be aggregated to fully aggregate and stabilize the impurity element tin. As shown in the photograph of the metallographic structure of a copper material to which a refining agent was added in FIG. 1, the compound of tin as an impurity element in copper and rare earth was present in the form of spherical particles in the interior of crystal grains as described in example 4, this is because the surface tension of the compound particle formed of rare earth and tin is larger than that of the copper melt, the particle morphology is spherical, however, because of the high viscosity of the copper solution, the buoyancy force of the compound particles formed by rare earth and tin in the solution is not enough to counteract the gravity force to float to the surface of the solution, so that the compound particles still exist in the copper matrix after solidification is finished, and the melting point of the compounds is higher than that of copper, so that the heterogeneous nucleation particles can be used as the centers of some heterogeneous nucleation particles during the solidification process and finally appear in the copper grains, rather than being concentrated at the grain boundaries, the refining agent is proved to be capable of effectively capturing low-content tin in the copper melt.
However, since the reaction product is a high-melting-point low-density compound, and the compound particles of rare earth and tin generated by low tin content are small, the buoyancy force applied to the copper melt with high viscosity is small, the copper melt is difficult to float to the surface of the copper melt to be removed as a slag phase against the self-gravity, and the impurity element tin still remains in the copper matrix in the form of a compound. Therefore, the deslagging agent is added on the basis, the deslagging agent is weakly alkaline, the rare earth and tin compounds are weakly acidic, and the deslagging agent can easily capture the rare earth and tin compounds generated in the melt under the interaction of acid and alkali, so that small compound particles grow up or are attached to the surface of the deslagging agent and float on the surface of the copper melt to be removed through slag removal, thereby thoroughly removing the impurity element tin in the copper melt and ensuring that the copper material has good electric conduction and heat conduction properties. Similarly, taking example 4 as an example, fig. 2 is a photograph of the metallographic structure of a copper material to which a refining agent and a slag removing agent have been added. The grain boundary and the inside of the crystal grain in the metallographic structure in the figure are very clean and have no impurities, which shows that the spherical compound particles formed by the rare earth and the tin are removed as a slag phase under the action of a deslagging agent, and correspondingly, the impurity element tin in the copper material is also removed.
It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be interchanged with other features disclosed in this application, but not limited to those having similar functions.
Claims (3)
1. A method for removing low-content impurity element tin in a copper melt comprises the following steps,
putting the copper material containing impurity element tin into a smelting furnace, controlling the temperature at 1150-1250 ℃ to completely melt the copper material into copper liquid, covering graphite powder covering agent with the thickness of 10-30 cm on the surface of the copper liquid in the melting process to pre-deoxidize and isolate air, obtaining copper melt after 30-60 minutes,
the method is characterized by further comprising the following steps:
secondly, wrapping the refining agent by using copper foil, pressing the refining agent into the copper melt by using a graphite bell jar to refine for 20 to 60 minutes,
and the content of the additive is calculated by weight percentage,
when the content of tin in the copper melt is 0.0003-0.03% and not including 0.03%, the refining agent is added in an amount of 0.01-0.1% and not including 0.1% of the copper melt,
when the content of tin in the copper melt is 0.03-1% and not 1%, the refining agent is added in an amount of 0.1-3% and not 3% of the copper melt,
when the tin content in the copper melt is 1-3%, the adding amount of the refining agent is 3-8% of the copper melt;
wherein the refining agent is intermediate alloy of rare earth elements of yttrium, praseodymium, neodymium, europium and copper, and is calculated by weight percentage,
1-20% of rare earth yttrium,
1 to 5 percent of praseodymium,
3-18% of neodymium,
2 to 15 percent of europium,
The balance being copper;
thirdly, adding a deslagging agent into the copper melt and stirring for 15-30 minutes, wherein the deslagging agent is added into every 100 grams of the copper melt by weight percent in a quantity of 3-8 grams, and then standing for 20-40 minutes and removing scum on the surface of the copper melt by using a slag spoon;
wherein the deslagging agent consists of sodium carbonate, sodium borate, sodium chloride and calcium fluoride in percentage by weight,
20-60% of sodium carbonate,
10-50% of sodium borate,
10-20% of sodium chloride,
5 to 20 percent of calcium fluoride,
The balance of inevitable impurities and the content of the impurities is 0 to 1 percent;
fourthly, pouring the copper melt after deslagging into a preheated mould to obtain the copper material with low melting point impurity element tin removed.
2. The method according to claim 1, wherein the refining agent has a particle size of 50-200 mesh.
3. The method as claimed in claim 1, wherein the size of the dross removal agent is 150-400 mesh.
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