Preparation process of high-activity copper oxide

The preparation of highly reactive copper oxide through biological materials and microwave treatment has solved the problem of insufficient specific surface area and poor activity of nano-scale copper oxide powder, and achieved a broader market application.

CN120328604APending Publication Date: 2025-07-18JIANGSU ZHIWEI NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202510551325.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-29
Publication Date
2025-07-18

AI Technical Summary

Technical Problem

In the prior art, the specific surface area of nano-scale copper oxide powder is insufficient and the activity performance is poor, which limits its application in cone materials and electronic materials.

Method used

Biomaterials are used to prepare auxiliary agents, and the high-active copper oxide product is prepared by microwave treatment and silane coupling agent treatment, combined with the mixing, drying and sintering of the copper source solution.

Benefits of technology

The specific surface area and active properties of copper oxide are improved, and its quality and quality are suitable for cone materials and electronic materials.

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Abstract

The invention relates to the technical field of copper oxide production, in particular to a preparation process of high-activity copper oxide. The auxiliary additive is prepared from a biological material, and is prepared by the following steps: mixing plant powder in a proper amount of triallyl isocyanurate solution, carrying out first microwave treatment on the obtained mixture in microwave treatment equipment, putting a silane coupling agent in a proper amount of the mixture, and carrying out second microwave treatment on the mixture in the microwave treatment equipment, so as to obtain the auxiliary additive. The preparation method comprises the following steps: preparing a copper source, placing the copper source in a microwave treatment device, carrying out second microwave treatment, carrying out suction filtration, washing, drying to obtain an auxiliary additive, preparing a base material solution from the copper source, placing the copper source in absolute ethyl alcohol, adding deionized water into the absolute ethyl alcohol to obtain the base material solution, placing the auxiliary additive in the base material solution, and fully mixing to obtain the copper-based composite material. And carrying out heat preservation, drying and sintering to finally prepare a high-activity copper oxide finished product. The prepared high-activity copper oxide not only has a relatively good specific area, but also has excellent activity, and the quality of the high-activity copper oxide is effectively ensured.
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Description

Technical Field

[0001] The present invention relates to the technical field of copper oxide production, and specifically to a preparation process of highly active copper oxide. Background Art

[0002] Copper oxide powder is soluble in acids, insoluble in water, alcohol, ammonium chloride and potassium cyanide solutions, slowly dissolves in ammonia solution, and can also react with strong alkalis. It is mainly used for preparing petroleum desulfurizers, catalysts, rayon, ceramics, pesticides, glass, etc. The active copper oxide powder with a nanoscale particle size has the advantages of rapid acid dissolution, fine particle size, low impurities, large specific surface area, high quality, strong activity, etc. Therefore, it has more advantages than ordinary copper oxide powder in printed circuits, especially in spray cone materials and electronic materials, where it has an irreplaceable role compared to ordinary copper oxide powder.

[0003] In the patent document with the application number "CN202110080050.5" and the name "A process for producing high-purity active copper oxide by complexation replacement method", it is recorded that "①. Prepare a copper sulfate solution in a reactor, heat it to 40 - 50 °C, slowly add the complexing agent ammonia water until complexation is complete, and make all the copper sulfate solution react to become copper ammonium complex salt; ②. Continue to heat to and maintain 70 - 75 °C, slowly add liquid alkali to make the pH value of the chemical solution reach 12 until oxidation is complete, and decompose the copper ammonium complex salt to obtain copper oxide; ③. Finally, boil for 2 - 3 hours to drive out the separated ammonia; ④. Use the filter cake for filtration to obtain copper oxide particles. After filtration, wash the filter cake with boiling water to wash away the sulfate radicals contained in the filter cake. ⑤. Dry the filter cake in an oven (90 - 110 °C), and then transfer it to a muffle furnace to bake for more than 3 hours to remove the substances that make the copper oxide active, and the finished product is obtained. The activity of the copper oxide obtained by this process technology can reach less than 20 s each time, the particles are uniform, loose and flowing, and the fineness of the copper oxide particles can reach more than 300 meshes". Although the copper oxide manufactured by this patent document has certain advantages such as activity, its specific surface area is relatively insufficient and still needs further improvement.

[0004] For another example, in the patent document with the application number "CN201711271156.3" and the title "Porous nano-copper oxide and its preparation method", it is recorded that "The preparation method of this porous nano-copper oxide is as follows: Dissolve the soluble salt and the swelling agent in deionized water, stir until completely dissolved, add the copper precursor to the obtained solution, stir until completely dissolved, place the obtained solution under dynamic conditions for hydrothermal crystallization, cool the solution to room temperature after hydrothermal treatment, filter, wash, dry, and calcine to obtain porous nano-copper oxide. The copper oxide prepared by the method of the present invention has the advantages of large specific surface area, adjustable pore channels, controllable thickness, good dispersibility, high thermal stability, and rich five-coordinated copper, etc. It can not only be used in the catalytic field, but also be applied to fields such as ceramics, coatings, and pigments after further subsequent high-temperature calcination to obtain copper oxide, etc.". Although the copper oxide manufactured by this patent document has advantages such as a large specific surface area, its own activity performance is not good.

[0005] Based on this, the present invention provides a preparation process of high-activity copper oxide to solve the above-mentioned technical problems! Summary of the Invention

[0006] The purpose of the present invention is to provide a preparation process of high-activity copper oxide. The prepared high-activity copper oxide not only has a good specific surface area, but also has excellent activity, effectively ensuring its quality and quality.

[0007] To achieve the above purpose, the present invention provides the following technical solutions: The present invention provides a preparation process of high-activity copper oxide, including the following steps: S1. Prepare an auxiliary additive using a biological material; S2. Prepare a base solution using a copper source; Among them, the process of preparing the base solution using the copper source is as follows: Place the copper source in absolute ethanol, stir at 450 - 650 r / min for 20 - 30 min, then add deionized water accounting for 50 - 60% of the mass of absolute ethanol, and continue stirring for 60 - 70 min to obtain the base solution; S3. Place the auxiliary additive in the base solution and mix well, and finally obtain the finished product of high-activity copper oxide after heat preservation, drying, and sintering; Among them, the temperature of the heat preservation is 60 - 70 °C, and the time is 100 - 120 min; The temperature of the drying is 70 - 80 °C, and the time is 80 - 100 min.

[0008] The present invention is further arranged as follows: In the step S1, the process of preparing the auxiliary additive using the biological material is as follows: Place the plant powder in an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 0.02 - 1.2 g / mL, and mix for 20 - 30 min under the condition of 120 - 220 r / min; After mixing, place the obtained mixture in a microwave treatment device for the first microwave treatment; Then, place the silane coupling agent in an appropriate amount of the mixture at a mass ratio of 0.02 - 0.08:1, mix for 5 - 10 min under the condition of 230 - 330 r / min, and then place it in a microwave treatment device for the second microwave treatment; After suction filtration, wash with absolute ethanol and deionized water 2 - 4 times respectively, and dry in an oven at 50 - 60 °C for 40 - 50 min to obtain the auxiliary additive.

[0009] A further setting of the present invention is that the plant powder is composed of pomelo peel powder and orange peel powder mixed at a mass ratio of 1:0.2 - 0.4.

[0010] A further setting of the present invention is that the triallyl isocyanurate solution is compounded from triallyl isocyanurate and absolute ethanol at a mass ratio of 0.08 - 0.24:1.

[0011] A further setting of the present invention is that the microwave frequency of the first microwave treatment is 2400 - 2420 MHz, the microwave power is 810 - 820 W, and the treatment time is 4 - 8 min.

[0012] A further setting of the present invention is that the silane coupling agent is selected from any one of silane coupling agent KH - 560 and silane coupling agent KH - 550.

[0013] A further setting of the present invention is that the microwave frequency of the second microwave treatment is 2200 - 2350 MHz, the microwave power is 800 - 810 W, and the treatment time is 3 - 7 min.

[0014] A further setting of the present invention is that in the step S2, the copper source is selected from any one of cupric nitrate trihydrate and copper acetate.

[0015] A further setting of the present invention is that in the step S3, the added mass ratio of the auxiliary additive and the base material solution is 0.13 - 0.33:1.

[0016] A further setting of the present invention is that in the step S3, the sintering is divided into two stages: The first stage: heat up to 400 - 410 °C at a heating rate of 8 - 10 °C / min and sinter for 20 - 30 min; The second stage: heat up to 455 - 465 °C at a heating rate of 2 - 5 °C / min and sinter for 30 - 40 min.

[0017] Compared with the prior art, the present invention has the following beneficial effects: The present invention adopts biomaterial to prepare auxiliary additives, wherein the auxiliary additives are plant powder placed in an appropriate amount of triallyl isocyanurate solution and mixed, and then the obtained mixture is placed in a microwave treatment device for a first microwave treatment, and then a silane coupling agent is placed in an appropriate amount of the mixture, and then placed in a microwave treatment device for a second microwave treatment, after filtration, washing, drying, obtaining the auxiliary additives, and then using a copper source to prepare a base material solution, wherein the base material solution is a copper source placed in anhydrous ethanol, and then deionized water is added thereto to obtain a base material solution, and finally the auxiliary additives are placed in the base material solution and fully mixed, and after heat preservation, drying, and sintering, a high-activity copper oxide finished product is finally prepared. The high-activity copper oxide prepared by the present invention not only has a good specific area, but also has excellent activity, and effectively guarantees its quality and quality. The preparation process of the high-activity copper oxide provided by the present invention has a broader market prospect and is more suitable for promotion. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] Embodiment 1: This embodiment provides a process for preparing highly active copper oxide, comprising the following steps: S1. Use biological materials to prepare auxiliary additives.

[0020] Among them, the process of using biological materials to prepare auxiliary additives is as follows: The plant powder was placed in an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 0.02 g / mL and mixed at 120 r / min for 20 min; After the mixing is completed, the obtained mixture is placed in a microwave treatment device for a first microwave treatment; Then, a silane coupling agent was placed in an appropriate amount of the mixture at a mass ratio of 0.02:1, mixed at 230 r / min for 5 min, and then placed in a microwave treatment device for a second microwave treatment; After filtration, the mixture was washed twice with anhydrous ethanol and deionized water respectively, and dried in a drying oven at 50° C. for 40 min to obtain an auxiliary agent.

[0021] Furthermore, the plant powder is prepared by mixing grapefruit peel powder and orange peel powder in a mass ratio of 1:0.2.

[0022] The triallyl isocyanurate solution is prepared by compounding triallyl isocyanurate and absolute ethanol according to a mass ratio of 0.08:1.

[0023] The microwave frequency of the first microwave treatment is 2400 MHz, the microwave power is 810 W, and the treatment time is 4 min.

[0024] The silane coupling agent selected is silane coupling agent KH-560.

[0025] The microwave frequency of the second microwave treatment is 2200 MHz, the microwave power is 800 W, and the treatment time is 3 min.

[0026] S2. Prepare the base material solution using a copper source; Among them, the process of preparing the base material solution using a copper source is as follows: Place the copper source in absolute ethanol, stir at 450 r / min for 20 min, then add deionized water accounting for 50% of the mass of absolute ethanol thereto, and continue stirring for 60 min to obtain the base material solution.

[0027] Furthermore, the copper source selected is copper nitrate trihydrate.

[0028] S3. Place the auxiliary additive in the base material solution and mix well. After heat preservation, drying, and sintering, finally prepare the high-activity copper oxide finished product; Among them, the heat preservation temperature is 60 °C and the time is 100 min; In addition, the mass ratio of the addition of the auxiliary additive to the base material solution is 0.13:1.

[0029] Furthermore, the sintering is divided into two stages: The first stage: Heat up to 400 °C at a heating rate of 8 °C / min and sinter for 20 min; The second stage: Heat up to 455 °C at a heating rate of 2 °C / min and sinter for 30 min.

[0030] Example 2: This example provides a preparation process for high-activity copper oxide, including the following steps: S1. Prepare the auxiliary additive using a biological material.

[0031] Among them, the process of preparing the auxiliary additive using a biological material is as follows: Place the plant powder in an appropriate amount of triallyl isocyanurate solution according to a dosage ratio of 0.04 g / mL, and mix at 122 r / min for 22 min; After mixing, place the obtained mixture in a microwave treatment device for the first microwave treatment; Then, place the silane coupling agent in an appropriate amount of the mixture at a mass ratio of 0.03:1, mix it at 232 r / min for 6 min, and then place it in a microwave treatment device for the second microwave treatment; After suction filtration, wash it 3 times with absolute ethanol and deionized water respectively, and dry it in a drying oven at 52 °C for 42 min to obtain the auxiliary additive.

[0032] Furthermore, the plant powder is composed of pomelo peel powder and orange peel powder mixed at a mass ratio of 1:0.3.

[0033] The triallyl isocyanurate solution is prepared by compounding triallyl isocyanurate and absolute ethanol at a mass ratio of 0.1:1.

[0034] The microwave frequency of the first microwave treatment is 2402 MHz, the microwave power is 812 W, and the treatment time is 5 min.

[0035] The silane coupling agent selected is silane coupling agent KH-550.

[0036] The microwave frequency of the second microwave treatment is 2210 MHz, the microwave power is 802 W, and the treatment time is 4 min.

[0037] S2. Prepare the base material solution using a copper source; Among them, the process of preparing the base material solution using a copper source is as follows: Place the copper source in absolute ethanol, stir it at 452 r / min for 22 min, then add deionized water accounting for 52% of the mass of absolute ethanol thereto, and continue stirring for 62 min to obtain the base material solution.

[0038] Furthermore, the copper source selected is copper acetate.

[0039] S3. Place the auxiliary additive in the base material solution and mix well. After heat preservation, drying, and sintering, finally prepare the high-activity copper oxide finished product; Among them, the heat preservation temperature is 62 °C and the time is 105 min; In addition, the added mass ratio of the auxiliary additive and the base material solution is 0.15:1.

[0040] Furthermore, the sintering is divided into two stages: The first stage: Heat it to 402 °C at a heating rate of 9 °C / min and sinter for 22 min; The second stage: Heat it to 457 °C at a heating rate of 3 °C / min and sinter for 32 min.

[0041] Example 3: This example provides a preparation process for high-activity copper oxide, including the following steps: S1. Prepare the auxiliary additive using biological materials.

[0042] Among them, the process of preparing the auxiliary additive using biological materials is as follows: Put the plant powder into an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 0.07 g / mL, and mix for 25 min under the condition of 170 r / min; After mixing, put the obtained mixture into a microwave treatment device for the first microwave treatment; Then, put the silane coupling agent into an appropriate amount of the mixture at a mass ratio of 0.06:1, mix for 7 min under the condition of 280 r / min, and then put it into the microwave treatment device for the second microwave treatment; After suction filtration, wash 3 times with absolute ethanol and deionized water respectively, and dry in a drying oven at 55 °C for 45 min to obtain the auxiliary additive.

[0043] Furthermore, the plant powder is composed of pomelo peel powder and orange peel powder mixed at a mass ratio of 1:0.3.

[0044] The triallyl isocyanurate solution is compounded by triallyl isocyanurate and absolute ethanol at a mass ratio of 0.16:1.

[0045] The microwave frequency of the first microwave treatment is 2410 MHz, the microwave power is 815 W, and the treatment time is 6 min.

[0046] The silane coupling agent selected is silane coupling agent KH-560.

[0047] The microwave frequency of the second microwave treatment is 2275 MHz, the microwave power is 805 W, and the treatment time is 5 min.

[0048] S2. Prepare the base material solution using a copper source; Among them, the process of preparing the base material solution using a copper source is as follows: Put the copper source into absolute ethanol, stir for 25 min under the condition of 500 r / min, then add deionized water accounting for 55% of the mass of absolute ethanol thereto, and continue stirring for 65 min to obtain the base material solution.

[0049] Furthermore, the copper source selected is copper nitrate trihydrate.

[0050] S3. Put the auxiliary additive into the base material solution and mix well. After heat preservation, drying, and sintering, finally obtain the finished product of highly active copper oxide; Among them, the heat preservation temperature is 65 °C and the time is 110 min; In addition, the added mass ratio of the auxiliary additive and the base material solution is 0.23:1.

[0051] Furthermore, the sintering is divided into two stages: The first stage: Heat up to 405 °C at a heating rate of 9 °C / min and sinter for 25 min; The second stage: Heat up to 460 °C at a heating rate of 3 °C / min and sinter for 35 min.

[0052] Example 4: This example provides a preparation process of highly active copper oxide, including the following steps: S1. Prepare an auxiliary additive using a biological material.

[0053] Among them, the process of preparing the auxiliary additive using a biological material is as follows: Place the plant powder in an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 0.1 g / mL and mix for 28 min under the condition of 210 r / min; After mixing, place the obtained mixture in a microwave treatment device for the first microwave treatment; Then place the silane coupling agent in an appropriate amount of the mixture at a mass ratio of 0.07:1 and mix for 9 min under the condition of 310 r / min, and then place it in a microwave treatment device for the second microwave treatment; After suction filtration, wash 3 times with absolute ethanol and deionized water respectively, and dry in a drying oven at 58 °C for 48 min to obtain the auxiliary additive.

[0054] Furthermore, the plant powder is composed of pomelo peel powder and orange peel powder mixed at a mass ratio of 1:0.3.

[0055] The triallyl isocyanurate solution is compounded from triallyl isocyanurate and absolute ethanol at a mass ratio of 0.22:1.

[0056] The microwave frequency of the first microwave treatment is 2410 MHz, the microwave power is 818 W, and the treatment time is 7 min.

[0057] The silane coupling agent selected is silane coupling agent KH-560.

[0058] The microwave frequency of the second microwave treatment is 2330 MHz, the microwave power is 808 W, and the treatment time is 6 min.

[0059] S2. Prepare a base solution using a copper source; Among them, the process of preparing the base solution using a copper source is as follows: Place the copper source in absolute ethanol, stir for 28 min under the condition of 640 r / min, and then add deionized water accounting for 58% of the mass of absolute ethanol thereto, and continue stirring for 68 min to obtain the base solution.

[0060] Furthermore, the copper source selected is copper nitrate trihydrate.

[0061] S3. Place the auxiliary additive in the base material solution and mix well. After heat preservation, drying, and sintering, finally obtain the finished product of highly active copper oxide; Among them, the heat preservation temperature is 68 °C and the time is 118 min; In addition, the added mass ratio of the auxiliary additive to the base material solution is 0.3:1.

[0062] Furthermore, the sintering is divided into two stages: The first stage: Heat up to 408 °C at a heating rate of 9 °C / min and sinter for 28 min; The second stage: Heat up to 462 °C at a heating rate of 4 °C / min and sinter for 38 min.

[0063] Example 5: This example provides a preparation process of highly active copper oxide, including the following steps: S1. Prepare the auxiliary additive using biological materials.

[0064] Among them, the process of preparing the auxiliary additive using biological materials is as follows: Place the plant powder in an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 1.2 g / mL, and mix for 30 min under the condition of 220 r / min; After mixing, place the obtained mixture in a microwave treatment device for the first microwave treatment; Then place the silane coupling agent in an appropriate amount of the mixture at a mass ratio of 0.08:1, mix for 10 min under the condition of 330 r / min, and then place it in a microwave treatment device for the second microwave treatment; After suction filtration, wash 4 times with anhydrous ethanol and deionized water respectively, and dry in an oven at 60 °C for 50 min to obtain the auxiliary additive.

[0065] Furthermore, the plant powder is composed of pomelo peel powder and orange peel powder mixed in a mass ratio of 1:0.4.

[0066] The triallyl isocyanurate solution is compounded by triallyl isocyanurate and anhydrous ethanol in a mass ratio of 0.24:1.

[0067] The microwave frequency of the first microwave treatment is 2420 MHz, the microwave power is 820 W, and the treatment time is 8 min.

[0068] The silane coupling agent is selected as silane coupling agent KH-560.

[0069] The microwave frequency of the second microwave treatment is 2350 MHz, the microwave power is 810 W, and the treatment time is 7 min.

[0070] S2. Prepare the base material solution using a copper source; Among them, the process of preparing the base material solution using a copper source is as follows: Place the copper source in absolute ethanol and stir it at 650 r / min for 30 min. Then add deionized water accounting for 60% of the mass of absolute ethanol to it and continue stirring for 70 min to obtain the base material solution.

[0071] Furthermore, the copper source is selected as copper nitrate trihydrate.

[0072] S3. Place the auxiliary additive in the base material solution for thorough mixing. After heat preservation, drying, and sintering, finally prepare the high-activity copper oxide finished product; Among them, the heat preservation temperature is 70 °C and the time is 120 min; In addition, the mass ratio of the addition of the auxiliary additive to the base material solution is 0.33:1.

[0073] Furthermore, the sintering is divided into two stages: The first stage: Heat up to 410 °C at a heating rate of 10 °C / min and sinter for 30 min; The second stage: Heat up to 465 °C at a heating rate of 5 °C / min and sinter for 40 min.

[0074] Comparative Example 1: The preparation method of the feed additive provided in this example, the specific ratio of raw materials, and Example 1 are substantially the same. The main difference is that in this example, an equal amount of wheat straw powder is used to replace the plant powder.

[0075] Comparative Example 2: The preparation method of the feed additive provided in this example, the specific ratio of raw materials, and Example 1 are substantially the same. The main difference is that in this example, an equal amount of corn straw powder is used to replace the plant powder.

[0076] Label the copper oxide samples provided in Examples 1 to 5 as Examples 1 to 5 respectively, and label the copper oxide samples prepared through Comparative Examples 1 to 2 as Comparative Examples 1 to 2; and conduct the following tests on the relevant properties of the copper oxide provided in Examples 1 to 5 and Comparative Examples 1 to 2 respectively: 1. Specific surface area test: The test method is to use a specific surface area analyzer BET (Nova 4000E) to measure the specific surface area of the sample.

[0077] 2. Activity test: The test method is to add 10.0 g of copper oxide powder to a 1000 mL solution prepared with 16 mL of sulfuric acid with a concentration of 98%, and record the time when the copper oxide powder is completely dissolved at room temperature.

[0078] The obtained test data are recorded in Table 1 and Table 2 below.

[0079]

[0080]

[0081] By comparing and analyzing the relevant data in Table 1 and Table 2, it can be seen that the highly active copper oxide prepared by the present invention not only has a good specific surface area, but also has excellent activity, effectively ensuring its quality and quality. This indicates that the preparation process of the highly active copper oxide provided by the present invention has a broader market prospect and is more suitable for popularization.

[0082] The present invention uses biological materials to prepare an auxiliary additive. The auxiliary additive is prepared by mixing plant powder in an appropriate amount of triallyl isocyanurate solution, then placing the obtained mixture in a microwave treatment device for the first microwave treatment, and then placing a silane coupling agent in an appropriate amount of the mixture and then placing it in a microwave treatment device for the second microwave treatment. After filtration, washing and drying, the auxiliary additive is obtained. Then, a base solution is prepared using a copper source. The base solution is prepared by placing the copper source in absolute ethanol and then adding deionized water thereto. Finally, the auxiliary additive is placed in the base solution and fully mixed. After heat preservation, drying and sintering, the finished product of highly active copper oxide is finally prepared. The highly active copper oxide prepared by the present invention not only has a good specific surface area, but also has excellent activity, effectively ensuring its quality and quality.

[0083] In the description of this specification, the descriptions referring to terms such as "one embodiment", "example", "specific example", etc. mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0084] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific embodiments described. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification in order to better explain the principles and practical applications of the present invention, so that those skilled in the relevant technical fields can understand and utilize the present invention well. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A preparation process of highly active copper oxide, characterized in that, The following steps are involved: S1. Using biological materials to prepare auxiliary additives; S2, using a copper source to prepare a base material solution; The process of preparing the base material solution using a copper source is as follows: The copper source is placed in anhydrous ethanol, stirred at 450-650 r / min for 20-30 min, and then deionized water with a mass ratio of 50-60% of the anhydrous ethanol is added thereto, and the stirring treatment is continued for 60-70 min to obtain a base material solution; S3, placing the auxiliary agent in the base material solution and mixing thoroughly, and finally preparing a high-activity copper oxide product after heat preservation, drying and sintering; Wherein, the temperature of the insulation is 60-70°C and the time is 100-120 minutes; The drying temperature is 70-80° C. and the drying time is 80-100 min.

2. The preparation process of a highly active copper oxide according to claim 1, characterized in that, In step S1, the process of preparing the auxiliary agent using biological materials is as follows: Place the plant powder in an appropriate amount of triallyl isocyanurate solution at a dosage ratio of 0.02 to 1.2 g / mL and mix at 120 to 220 r / min for 20 to 30 minutes; After the mixing is completed, the obtained mixture is placed in a microwave treatment device for a first microwave treatment; Then, a silane coupling agent is placed in an appropriate amount of the mixture at a mass ratio of 0.02 to 0.08:1, mixed at 230 to 330 r / min for 5 to 10 minutes, and then placed in a microwave treatment device for a second microwave treatment; After filtration, the product is washed with anhydrous ethanol and deionized water for 2 to 4 times respectively, and dried in a drying oven at 50 to 60° C. for 40 to 50 minutes to obtain an auxiliary agent.

3. The preparation process of a highly active copper oxide according to claim 2, characterized in that, The plant powder is prepared by mixing grapefruit peel powder and orange peel powder in a mass ratio of 1:0.2-0.

4.

4. A preparation process of highly active copper oxide according to claim 2, characterized in that, The triallyl isocyanurate solution is prepared by compounding triallyl isocyanurate and anhydrous ethanol in a mass ratio of 0.08 to 0.24:

1.

5. The preparation process of a highly active copper oxide according to claim 2, wherein The microwave frequency of the first microwave treatment is 2400-2420 MHz, the microwave power is 810-820 W, and the treatment time is 4-8 min.

6. The preparation process of a highly active copper oxide according to claim 2, characterized in that, The silane coupling agent is selected from any one of silane coupling agent KH-560 and silane coupling agent KH-550.

7. A preparation process of highly active copper oxide according to claim 2, characterized in that: The microwave frequency of the second microwave treatment is 2200-2350 MHz, the microwave power is 800-810 W, and the treatment time is 3-7 minutes.

8. A preparation process of highly active copper oxide according to claim 1, characterized in that, In step S2, the copper source is selected from any one of copper nitrate trihydrate and copper acetate.

9. A preparation process of high-activity copper oxide according to claim 1, characterized in that, In the step S3, the mass ratio of the auxiliary agent to the base material solution is 0.13-0.33:

1.

10. A preparation process of high-activity copper oxide according to claim 1, characterized in that, In step S3, the sintering is divided into two stages: The first stage: heating to 400-410°C at a heating rate of 8-10°C / min and sintering for 20-30 minutes; The second stage: heating to 455-465°C at a heating rate of 2-5°C / min and sintering for 30-40 minutes.

Citation Information

Patent Citations

  • Porous nanometer copper oxide and preparation method thereof

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    CN112897566A