Antioxidant copper rod and preparation method thereof
By coating and heating the antioxidant coating liquid on the surface of the copper rod to form an antioxidant film, the problem of poor oxidation resistance of existing copper rods is solved, and the antioxidant performance and service life of the copper rods are significantly improved.
Patent Information
- Application Number
- CN202510220824.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-27
- Publication Date
- 2025-05-13
- Estimated Expiration
- 2045-02-27
AI Technical Summary
The poor oxidation resistance of existing copper rods leads to the formation of copper rust affects the conductivity and mechanical strength, reducing service life and product reliability.
The antioxidant coating liquid is used to coat the copper rod surface and heat-cured to form an antioxidant film. The antioxidant coating liquid consists of epoxy resin, antioxidant, filler, anti-ultraviolet agent, curing agent, leveling agent and solvent. Antioxidants significantly enhance the antioxidant effect through the mercapto-click reaction and the multifunctional group.
It significantly improves the oxidation resistance of copper rods, extends service life, enhances conductive properties and mechanical strength, and meets the market demand for high quality and high performance.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of metal coatings, and more specifically, to an anti-oxidation copper rod and a preparation method thereof. Background Art
[0002] In modern industrial production, copper rods, as a basic metal material, have been widely used in many fields such as electricity, electronics, and construction due to their good electrical conductivity, thermal conductivity, and processing performance. From cable manufacturing in power transmission, to precision components in electronic equipment, to water supply and drainage pipes in the construction field, copper rods play an indispensable role.
[0003] However, the copper rods currently on the market generally have poor antioxidant properties. Copper easily reacts chemically with oxygen in the air to form copper rust. The appearance of copper rust not only affects the appearance of the copper rod, making its surface lose its luster and appear mottled rust, but more seriously, it greatly reduces the performance of the copper rod. On the one hand, the presence of copper rust will increase the resistance of the copper rod, thereby affecting its conductivity, reducing power transmission efficiency, and increasing energy loss. In the power system, this may lead to increased voltage drop, waste of electrical energy, and even cause safety hazards. On the other hand, copper rust will weaken the mechanical strength of the copper rod, making it more prone to breakage during processing and use, reducing the reliability and service life of the product.
[0004] As various industries have increasingly higher requirements for the quality and performance of copper rods, various industries have put forward higher and higher requirements for the quality and performance of copper rods. However, the existing copper rods are unable to meet the growing market demand due to their insufficient anti-oxidation performance; therefore, the present application provides an anti-oxidation copper rod and a preparation method thereof. Summary of the invention
[0005] In order to solve the problem that the existing copper rod has poor anti-oxidation effect, the present application provides an anti-oxidation copper rod and a preparation method thereof.
[0006] In a first aspect, the present application provides a method for preparing an oxidation-resistant copper rod, using the following technical solution: A method for preparing an oxidation-resistant copper rod comprises the following steps: After the anti-oxidation coating liquid is coated on the surface of the copper rod, a heating and curing treatment is performed to form an anti-oxidation film on the surface of the copper rod; The anti-oxidation coating liquid comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 20-30 parts of antioxidant, 15-20 parts of filler, 1-10 parts of anti-ultraviolet agent, 5-10 parts of curing agent, 1-5 parts of leveling agent and 20-40 parts of solvent.
[0007] Preferably, the method for preparing the antioxidant comprises the following steps: S1. Add octamethylcyclotetrasiloxane, 3-mercaptopropylmethyldimethoxysilane, hexamethyldisiloxane and concentrated sulfuric acid into water, stir evenly at room temperature, react in an oil bath at 60-70°C for 8-12h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2. Add the mercapto silicone oil, 4-allylcatechol, eugenol and benzophenone obtained in step S1 into toluene, mix evenly, irradiate under ultraviolet light for 1-3 hours, concentrate under reduced pressure, wash, add anhydrous magnesium sulfate to dry, filter, and rotary evaporate to obtain an antioxidant.
[0008] Preferably, the mass ratio of octamethylcyclotetrasiloxane, 3-mercaptopropylmethyldimethoxysilane, hexamethyldisiloxane, concentrated sulfuric acid and water in step S1 is (59-65) g: (36-40) g: (16-20) g: (1.6-2) g: (200-400) g.
[0009] Preferably, the mass ratio of the mercapto silicone oil, 4-allylcatechol, eugenol, benzophenone and toluene in step S2 is (50-60) g: (7.5-8) g: (8-8.5) g: (1-1.5) g: (200-400) g.
[0010] Preferably, the filler is obtained by mixing nano yttrium oxide and nano tantalum oxide in a mass ratio of 3:(1-7).
[0011] Preferably, the anti-ultraviolet agent is at least one of UV-320, UV-531, UV-328, UV-1130, UV-326, UV-123, and UV-400.
[0012] Preferably, the curing agent is at least one of maleic anhydride, phthalic anhydride, m-phenylenediamine, diethylenetriamine, ethylenediamine, and phenylenediamine.
[0013] Preferably, the leveling agent is at least one of BYK-333, BYK-332, and BYK-3560.
[0014] Preferably, the solvent is at least one of ethanol, butanone, xylene, and ethylene glycol monobutyl ether.
[0015] In a second aspect, the present application provides an anti-oxidation copper rod, which adopts the following technical solution: An oxidation-resistant copper rod is prepared by the above-mentioned preparation method.
[0016] In summary, this application has the following beneficial effects: 1. The antioxidant film on the surface of the copper rod of the present application is formed by heating and curing the antioxidant coating liquid. The antioxidant coating liquid includes epoxy resin, antioxidant, filler, anti-ultraviolet agent, curing agent, leveling agent, and solvent. The components interact with each other, and the obtained copper rod has excellent antioxidant properties, which effectively prolongs the service life of the copper rod, improves its comprehensive performance, and meets the high quality and high performance requirements of copper rods in different industries.
[0017] 2. In the preparation process of the antioxidant of the present application, first, under the catalysis of concentrated sulfuric acid, the siloxy bond of octamethylcyclotetrasiloxane undergoes a ring-opening reaction, and at the same time, the methoxy group of 3-mercaptopropylmethyldimethoxysilane is hydrolyzed to generate a hydroxyl group; the ring-opened octamethylcyclotetrasiloxane and the hydrolyzed 3-mercaptopropylmethyldimethoxysilane are connected through a condensation reaction of the siloxy bond, and the siloxy bond in hexamethyldisiloxane is broken and connected to one end of the polymer chain to obtain mercapto silicone oil. The siloxy bond in the mercapto silicone oil has a high bond energy and stable chemical properties, and can provide a stable skeleton for the entire antioxidant molecule. The framework structure can ensure that the antioxidant can maintain its molecular integrity under various complex environmental conditions, thereby continuously exerting its antioxidant effect; then the mercapto group in the mercapto silicone oil can react with the carbon-carbon double bonds in 4-allylcatechol and eugenol under the action of the initiator to undergo a thiol click reaction to obtain antioxidants. The molecules of 4-allylcatechol and eugenol contain multiple phenolic hydroxyl groups with hydrogen-donating capacity. In the antioxidant process, the phenolic hydroxyl groups can provide hydrogen atoms to combine with free radicals, converting the free radicals into stable molecules, thereby interrupting the free radical chain reaction and achieving the purpose of antioxidant.
[0018] The antioxidant of the present application greatly enhances the antioxidant effect of the antioxidant by virtue of its stable molecular structure and synergistic effect of multiple functional groups, so that it can more effectively remove various types of free radicals and protect the copper rod from oxidative damage.
[0019] 3. The filler of the present application is obtained by mixing nano yttrium oxide and nano tantalum oxide. When it is evenly dispersed in the anti-oxidation coating liquid and coated on the surface of the copper rod to form a thin film, it can be closely arranged to form a dense and continuous protective layer. Nano yttrium oxide and nano tantalum oxide, the two synergistically enhance each other, can interact with antioxidants to enhance their antioxidant effect; on the one hand, the surface of the nano material can adsorb antioxidant molecules, so that the antioxidants are more evenly distributed in the coating and improve their utilization rate; on the other hand, nano yttrium oxide and nano tantalum oxide will also affect the electronic structure of the antioxidant molecules, enhance the hydrogen supply capacity of phenolic hydroxyl and thiol, thereby more effectively enhancing the antioxidant performance of the copper rod.
[0020] 4. The preparation method of the antioxidant copper rod of the present application has simple steps, low cost, is suitable for industrial production, effectively solves the problem of poor antioxidant performance of existing copper rods, and has broad application prospects. DETAILED DESCRIPTION
[0021] The present application is further described in detail below with reference to the embodiments.
[0022] Embodiment 1-5 provides a method for preparing an oxidation-resistant copper rod.
[0023] Embodiment 1:
[0024] A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 59 g of octamethylcyclotetrasiloxane, 36 g of 3-mercaptopropylmethyldimethoxysilane, 16 g of hexamethyldisiloxane and 1.6 g of concentrated sulfuric acid (98 wt%) to 200 g of water, stir evenly at room temperature, react in an oil bath at 60 ° C for 8 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 50 g of the mercapto silicone oil obtained in step S1, 7.5 g of 4-allyl catechol, 8 g of eugenol, and 1 g of benzophenone to 200 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:1; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; and the solvent is ethanol; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0025] Embodiment 2:
[0026] A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 61 g of octamethylcyclotetrasiloxane, 38 g of 3-mercaptopropylmethyldimethoxysilane, 18 g of hexamethyldisiloxane and 1.7 g of concentrated sulfuric acid (98 wt%) to 250 g of water, stir evenly at room temperature, react in an oil bath at 62 ° C for 9 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 52 g of mercapto silicone oil obtained in step S1, 7.6 g of 4-allyl catechol, 8.2 g of eugenol, and 1.2 g of benzophenone to 250 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1.5 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 22 parts of antioxidant, 16 parts of filler, 3 parts of anti-ultraviolet agent, 7 parts of curing agent, 2 parts of leveling agent and 25 parts of solvent were mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:2; the anti-ultraviolet agent is UV-531; the curing agent is phthalic anhydride; the leveling agent is BYK-332; and the solvent is butanone; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 110° C. and a pressure of 2.5 MPa for 1.8 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0027] Embodiment 3:
[0028] A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 63 g of octamethylcyclotetrasiloxane, 38 g of 3-mercaptopropylmethyldimethoxysilane, 18 g of hexamethyldisiloxane and 1.8 g of concentrated sulfuric acid (98 wt%) to 300 g of water, stir evenly at room temperature, react in an oil bath at 65 °C for 10 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 55 g of the mercapto silicone oil obtained in step S1, 7.8 g of 4-allyl catechol, 8.3 g of eugenol, and 1.3 g of benzophenone to 300 g of toluene, uniformly mixing, irradiating under ultraviolet light for 2 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 25 parts of antioxidant, 18 parts of filler, 5 parts of anti-ultraviolet agent, 8 parts of curing agent, 2.5 parts of leveling agent and 30 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:5; the anti-ultraviolet agent is UV-1130; the curing agent is ethylenediamine; the leveling agent is BYK-3560; and the solvent is xylene. Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 130° C. and a pressure of 3 MPa for 1.5 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0029] Embodiment 4:
[0030] A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 63 g of octamethylcyclotetrasiloxane, 39 g of 3-mercaptopropylmethyldimethoxysilane, 19 g of hexamethyldisiloxane and 1.8 g of concentrated sulfuric acid (98 wt%) to 350 g of water, stir evenly at room temperature, react in an oil bath at 68 ° C for 11 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 58 g of mercapto silicone oil obtained in step S1, 7.8 g of 4-allyl catechol, 8.4 g of eugenol, and 1.4 g of benzophenone to 350 g of toluene, uniformly mixing, irradiating under ultraviolet light for 2.5 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 28 parts of antioxidant, 18 parts of filler, 8 parts of anti-ultraviolet agent, 9 parts of curing agent, 4 parts of leveling agent and 35 parts of solvent were mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 1:2; the anti-ultraviolet agent is UV-320; the curing agent is diethylenetriamine; the leveling agent is BYK-333; and the solvent is xylene; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 140° C. and a pressure of 3.5 MPa for 1.2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0031] Embodiment 5:
[0032] A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 65 g of octamethylcyclotetrasiloxane, 40 g of 3-mercaptopropylmethyldimethoxysilane, 20 g of hexamethyldisiloxane and 2 g of concentrated sulfuric acid (98 wt%) to 400 g of water, stir evenly at room temperature, react in an oil bath at 70 ° C for 12 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 60 g of the mercapto silicone oil obtained in step S1, 8 g of 4-allyl catechol, 8.5 g of eugenol, and 1.5 g of benzophenone to 400 g of toluene, uniformly mixing, irradiating under ultraviolet light for 3 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, filtering, and rotary evaporating to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 30 parts of antioxidant, 20 parts of filler, 10 parts of anti-ultraviolet agent, 10 parts of curing agent, 5 parts of leveling agent and 40 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is obtained by mixing nano yttrium oxide and nano tantalum oxide in a mass ratio of 3:7; the anti-ultraviolet agent is obtained by mixing UV-320 and UV-326 in a mass ratio of 2:1; the curing agent is obtained by mixing maleic anhydride and ethylenediamine in a mass ratio of 1:1; the leveling agent is BYK-333; and the solvent is ethanol. Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 150° C. and a pressure of 4 MPa for 1 hour to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0033] In order to verify the comprehensive performance of the anti-oxidation copper rods obtained in Examples 1-5 of the present application, the applicant set up Comparative Examples 1-5, which are as follows: Comparative Example 1 Comparative Example 1 is different from Example 1 only in that an equal amount of 4-allylcatechol is used to replace eugenol, as follows: A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 59 g of octamethylcyclotetrasiloxane, 36 g of 3-mercaptopropylmethyldimethoxysilane, 16 g of hexamethyldisiloxane and 1.6 g of concentrated sulfuric acid (98 wt%) to 200 g of water, stir evenly at room temperature, react in an oil bath at 60 ° C for 8 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 50 g of the mercapto silicone oil obtained in step S1, 15.5 g of 4-allyl catechol, and 1 g of benzophenone to 200 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, filtering, and rotary evaporating to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:1; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; and the solvent is ethanol; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0034] Comparative Example 2 Comparative Example 2 is different from Example 1 only in that 4-allylcatechol is replaced with an equal mass of eugenol, as follows: A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 59 g of octamethylcyclotetrasiloxane, 36 g of 3-mercaptopropylmethyldimethoxysilane, 16 g of hexamethyldisiloxane and 1.6 g of concentrated sulfuric acid (98 wt%) to 200 g of water, stir evenly at room temperature, react in an oil bath at 60 ° C for 8 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 50 g of the mercapto silicone oil obtained in step S1, 15.5 g of eugenol, and 1 g of benzophenone to 200 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, filtering, and rotary evaporating to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:1; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; and the solvent is ethanol; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0035] Comparative Example 3 Comparative Example 3 is different from Example 1 only in that the antioxidant is antioxidant 1010, specifically as follows: A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; The epoxy resin is E-51; the antioxidant is antioxidant 1010; the filler is a mixture of nano-yttrium oxide and nano-tantalum oxide in a mass ratio of 3:1; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; and the solvent is ethanol; Step (2) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0036] Comparative Example 4 Comparative Example 4 is different from Example 1 only in that the filler is nano yttrium oxide, as follows: A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 59 g of octamethylcyclotetrasiloxane, 36 g of 3-mercaptopropylmethyldimethoxysilane, 16 g of hexamethyldisiloxane and 1.6 g of concentrated sulfuric acid (98 wt%) to 200 g of water, stir evenly at room temperature, react in an oil bath at 60 ° C for 8 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 50 g of the mercapto silicone oil obtained in step S1, 7.5 g of 4-allyl catechol, 8 g of eugenol, and 1 g of benzophenone to 200 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; Among them, the epoxy resin is E-51; the filler is nano yttrium oxide; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; the solvent is ethanol; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0037] Comparative Example 5 Comparative Example 5 is different from Example 1 only in that the filler is nano tantalum oxide, specifically as follows: A method for preparing an oxidation-resistant copper rod comprises the following steps: Step (1) Preparation of antioxidant S1. Add 59 g of octamethylcyclotetrasiloxane, 36 g of 3-mercaptopropylmethyldimethoxysilane, 16 g of hexamethyldisiloxane and 1.6 g of concentrated sulfuric acid (98 wt%) to 200 g of water, stir evenly at room temperature, react in an oil bath at 60 ° C for 8 h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2, adding 50 g of the mercapto silicone oil obtained in step S1, 7.5 g of 4-allyl catechol, 8 g of eugenol, and 1 g of benzophenone to 200 g of toluene, uniformly mixing, irradiating under ultraviolet light for 1 h, concentrating under reduced pressure, washing, adding anhydrous magnesium sulfate to dry, suction filtering, and rotary evaporation to obtain an antioxidant; Step (2) Preparation of anti-oxidation coating liquid By weight, 100 parts of epoxy resin, 20 parts of antioxidant, 15 parts of filler, 1 part of anti-ultraviolet agent, 5 parts of curing agent, 1 part of leveling agent and 20 parts of solvent are mixed evenly to obtain an anti-oxidation coating liquid; Among them, the epoxy resin is E-51; the filler is nano-tantalum oxide; the anti-ultraviolet agent is UV-320; the curing agent is maleic anhydride; the leveling agent is BYK-333; the solvent is ethanol; Step (3) Preparation of Anti-Oxidation Copper Rod After the anti-oxidation coating liquid is coated on the surface of the copper rod, it is heated and cured at a temperature of 100° C. and a pressure of 2 MPa for 2 hours to form an anti-oxidation film on the surface of the copper rod to obtain an anti-oxidation copper rod.
[0038] The comprehensive properties of the antioxidant copper rods obtained in Examples 1-5 of the present application and Comparative Examples 1-5 were tested respectively, and the test results are shown in Table 1 below.
[0039] (1) According to GB / T1865-1997 "Artificial Weathering and Artificial Radiation Exposure of Paints and Varnishes", the antioxidant copper rods prepared in Examples 1-5 and Comparative Examples 1-5 were subjected to an artificial weathering test for 1500 hours; (2) After the anti-oxidation copper rods prepared in Examples 1-5 and Comparative Examples 1-5 were kept at 200°C for 15 minutes, a hot and cold alternating test was performed, and after 150 repetitions, whether cracks were generated was detected; then, after keeping at 250°C for 15 minutes, a hot and cold alternating test was performed, and after 50 repetitions, whether cracks were generated was detected; then, after keeping at 300°C for 15 minutes, a hot and cold alternating test was performed, and after 30 repetitions, whether cracks were generated was detected; (3) The water resistance (25°C, 300h) of the antioxidant copper rods prepared in Examples 1-5 and Comparative Examples 1-5 was tested in accordance with GB 5209-1985 "Determination of water resistance of paints and varnishes - Immersion method" with the test standard being no blistering and no rusting.
[0040] Table 1:
[0041] It can be seen from the data shown in Table 1 above that the antioxidant film on the surface of the antioxidant copper rod obtained in Examples 1-5 has good adhesion, dense structure, and durability compared with Comparative Examples 1-5, and has excellent antioxidant performance, high temperature resistance and water resistance, is green and environmentally friendly, and has broad market prospects.
[0042] The antioxidant coating liquid used for the copper rod in Example 1 contains 4-allylcatechol and eugenol as the raw materials for preparing the antioxidant. Compared with Comparative Examples 1 and 2, it is fully demonstrated that there is interaction and synergistic effect between 4-allylcatechol and eugenol, which greatly improves the antioxidant performance of the copper rod.
[0043] The antioxidant coating liquid used for the copper rod in Example 1, the raw materials for preparing the antioxidant include octamethylcyclotetrasiloxane, 3-mercaptopropylmethyldimethoxysilane, hexamethyldisiloxane, 4-allylcatechol and eugenol. Compared with Comparative Example 3, it is fully demonstrated that the antioxidant of the present application can significantly enhance the antioxidant properties of the copper rod.
[0044] The filler of the anti-oxidation coating liquid used for the copper rod in Example 1 is obtained by mixing nano yttrium oxide and nano tantalum oxide. Compared with Comparative Examples 4 and 5, it is fully demonstrated that nano yttrium oxide and nano tantalum oxide work synergistically to improve the anti-oxidation performance, high temperature resistance and water resistance of the copper rod.
[0045] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.
Claims
1. A method for preparing an oxidation-resistant copper rod, characterized in that: The following steps are involved: After the anti-oxidation coating liquid is coated on the surface of the copper rod, a heating and curing treatment is performed to form an anti-oxidation film on the surface of the copper rod; The anti-oxidation coating liquid comprises the following raw materials in parts by weight: 100 parts of epoxy resin, 20-30 parts of antioxidant, 15-20 parts of filler, 1-10 parts of anti-ultraviolet agent, 5-10 parts of curing agent, 1-5 parts of leveling agent and 20-40 parts of solvent.
2. The method for preparing an anti-oxidation copper rod according to claim 1, characterized in that: The preparation method of the antioxidant comprises the following steps: S1. Add octamethylcyclotetrasiloxane, 3-mercaptopropylmethyldimethoxysilane, hexamethyldisiloxane and concentrated sulfuric acid into water, stir evenly at room temperature, react in an oil bath at 60-70°C for 8-12h under nitrogen protection, cool to room temperature, add excess calcium hydroxide to the reaction solution to neutralize the concentrated sulfuric acid, filter, add excess anhydrous magnesium sulfate to the obtained filtrate, dry, filter with suction, and rotary evaporate to obtain mercapto silicone oil; S2. Add the mercapto silicone oil, 4-allylcatechol, eugenol and benzophenone obtained in step S1 into toluene, mix evenly, irradiate under ultraviolet light for 1-3 hours, concentrate under reduced pressure, wash, add anhydrous magnesium sulfate to dry, filter, and rotary evaporate to obtain an antioxidant.
3. The method for preparing an anti-oxidation copper rod according to claim 2, characterized in that: The mass ratio of octamethylcyclotetrasiloxane, 3-mercaptopropylmethyldimethoxysilane, hexamethyldisiloxane, concentrated sulfuric acid and water in step S1 is (59-65) g: (36-40) g: (16-20) g: (1.6-2) g: (200-400) g.
4. The method for preparing an anti-oxidation copper rod according to claim 2, characterized in that: The mass ratio of the mercapto silicone oil, 4-allylcatechol, eugenol, benzophenone and toluene in step S2 is (50-60) g: (7.5-8) g: (8-8.5) g: (1-1.5) g: (200-400) g.
5. The method for preparing an oxidation-resistant copper rod according to claim 1, characterized in that: The filler is obtained by mixing nano yttrium oxide and nano tantalum oxide in a mass ratio of 3:(1-7).
6. The method for preparing an oxidation-resistant copper rod according to claim 1, characterized in that: The anti-ultraviolet agent is at least one of UV-320, UV-531, UV-328, UV-1130, UV-326, UV-123, and UV-400.
7. The method for preparing an oxidation-resistant copper rod according to claim 1, characterized in that: The curing agent is at least one of maleic anhydride, phthalic anhydride, m-phenylenediamine, diethylenetriamine, ethylenediamine and phenylenediamine.
8. The method for preparing an oxidation-resistant copper rod according to claim 1, characterized in that: The leveling agent is at least one of BYK-333, BYK-332 and BYK-3560.
9. The method for preparing an anti-oxidation copper rod according to claim 1, characterized in that: The solvent is at least one of ethanol, butanone, xylene and ethylene glycol monobutyl ether.
10. An anti-oxidation copper rod prepared by the preparation method according to any one of claims 1 to 9.
Citation Information
Patent Citations
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