Production process of diuron
By using nitrogen-doped cobalt-selenium oxide catalysts supported by magnetic carbon nanotubes, the problems of low efficiency and harsh reaction conditions of traditional catalysts are solved, and efficient production of Dicaolong is achieved, which improves yield and purity and reduces production costs.
Patent Information
- Application Number
- CN202510455406.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-11
- Publication Date
- 2025-07-11
AI Technical Summary
The catalytic efficiency of traditional catalysts is low, the reaction conditions are harsh and the product separation is difficult, resulting in low production efficiency and high cost, making it difficult to meet industrial needs.
The cobalt selenium oxide Co3O4-SeO2/N-MCNTs supported by nitrogen-doped magnetic carbon nanotubes are used as catalysts to produce dicaolon through addition reactions, using its high specific surface area and unique structure to improve the dispersion and stability of the catalyst, avoid side reactions, and achieve magnetic separation.
The reaction rate is accelerated, the yield and purity of Dicaolong is improved, the production cost is reduced, and the product separation process is simplified.
Smart Images
Figure BDA0005355334410000081 
Figure BDA0005355334410000091
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of diuron synthesis, and particularly relates to a production process of diuron. Background Art
[0002] Diuron, with the chemical name of N-(3,4-dichlorophenyl)-N',N'-dimethylurea and the molecular formula of C9H 10 Cl2N2O, is a highly efficient and broad-spectrum urea herbicide. It effectively controls weeds in fields, orchards, tea gardens and other areas by inhibiting electron transfer in plant photosynthesis, and has important agricultural application value. However, the traditional production process of diuron has problems such as low production efficiency, harsh reaction conditions, and difficult product separation, which limit its large-scale industrial production and application.
[0003] Currently, the synthesis of diuron mainly adopts the addition reaction of 3,4-dichlorophenyl isocyanate and dimethylamine. A catalyst can be selected to accelerate the reaction process. Traditional catalysts include organic bases (such as triethylamine, pyridine) and metal salts (such as zinc chloride, zinc acetate), etc. Although they can catalyze the reaction, they have the following limitations: (1) Low catalytic efficiency: The activity of traditional catalysts is low, resulting in long reaction time and low conversion rate, which is difficult to meet the requirements of industrial production; (2) Harsh reaction conditions: Some catalysts require high temperature, high pressure and other conditions, increasing energy consumption and production costs; (3) Difficult product separation: It is difficult to separate the catalyst from the product, resulting in low product purity, complex subsequent treatment, and affecting product quality.
[0004] In the aqueous phase reaction system, the stability and dispersibility of the catalyst have an important impact on the reaction efficiency. Traditional catalysts are prone to deactivation or agglomeration in the aqueous phase, resulting in a decrease in catalytic efficiency. Therefore, the development of efficient catalysts has become an important direction for the improvement of the diuron production process. Summary of the Invention
[0005] The present invention provides a production process of diuron, which can solve the problem of low catalytic efficiency existing in the process of catalytic production of diuron in the prior art.
[0006] A production process of diuron, the specific steps include: adding 3,4-dichlorophenyl isocyanate, toluene and a catalyst into a reaction kettle for mixing, heating to 22-24°C, adding an aqueous solution of dimethylamine, heating to 40-50°C for reaction, cooling to room temperature, keeping warm for 0.5-1 h, and obtaining diuron after centrifugation, washing and drying;
[0007] The catalyst is cobalt selenide oxide supported on nitrogen-doped magnetic carbon nanotubes, represented as Co3O4-SeO2 / N-MCNTs.
[0008] Further, the weight ratio of the amounts of 3,4-dichlorophenyl isocyanate, toluene, and aqueous dimethylamine solution is 20-25:100:2-3.
[0009] Further, the amount of the catalyst used is 3-5% of the mass of 3,4-dichlorophenyl isocyanate.
[0010] Further, the mass fraction of the aqueous dimethylamine solution is 50-55%.
[0011] Further, the catalyst Co3O4-SeO2 / N-MCNTs is prepared by the following steps:
[0012] Dissolve cobalt chloride hexahydrate, selenium nitrate, and sodium acetate anhydride in an ethylene glycol solution, add nitrogen-doped magnetic carbon nanotubes and soak for 8-10 h, then react at 200-220 °C for 10-12 h. After the reaction is completed, wash the sample with absolute ethanol and deionized water and dry it to obtain Co3O4-SeO2 / N-MCNTs.
[0013] Further, the weight ratio of the amounts of cobalt chloride hexahydrate, selenium nitrate, sodium acetate anhydride, nitrogen-doped magnetic carbon nanotubes, and ethylene glycol solution is 5:5:1:0.6-1:60.
[0014] Further, the mass fraction of the ethylene glycol solution is 60-70%.
[0015] Further, the nitrogen-doped magnetic carbon nanotubes are prepared by the following steps:
[0016] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic treatment, then add melamine and disperse it by ultrasonic treatment to form a solution; continuously stir the solution at 70-75 °C until the ethanol completely evaporates to obtain a precursor; dry and grind the precursor, and then place it in a tubular furnace filled with Ar gas and perform high-temperature calcination pyrolysis according to the set heating program to obtain nitrogen-doped magnetic carbon nanotubes.
[0017] Further, the molar ratio of ferric chloride hexahydrate to melamine is 1:2.
[0018] Further, the set heating program is: raise the furnace temperature to 650-850 °C at a rate of 3 °C / min and hold for 2 h.
[0019] Advantages of the present invention:
[0020] (1) In the present invention, Co3O4-SeO2 / N-MCNTs is used to catalyze the production of diuron from 3,4-dichlorophenyl isocyanate and aqueous dimethylamine solution, which can accelerate the reaction rate, improve the yield and purity. The reasons are as follows:
[0021] 1) Nitrogen-doped magnetic carbon nanotubes have a high specific surface area and a unique tubular structure. As a carrier, Co3O4 and SeO2 can be uniformly dispersed on its surface or inside, improving the dispersion and stability of the catalyst. Due to the coordination effect between nitrogen-doped magnetic carbon nanotubes and Co ions, and the synergistic effect between Co3O4 and SeO2, Co3O4 and SeO2 can be anchored on nitrogen-doped magnetic carbon nanotubes, making Co3O4 and SeO2 not easily fall off or break during the catalytic process. The catalyst not only has abundant active sites but also good chemical stability.
[0022] 2) Nitrogen-doped magnetic carbon nanotubes have a high specific surface area and can dynamically adsorb water molecules during the reaction process, effectively avoiding the side reaction of hydrolysis of 3,4-dichlorophenyl isocyanate to form N,N-bis(3,4-dichlorophenyl)urea.
[0023] Therefore, the abundant active sites of the catalyst, good chemical stability, and effective avoidance of side reactions can improve the yield and purity of diuron.
[0024] (2) The Co3O4-SeO2 / N-MCNTs catalyst used in the present invention not only has high catalytic efficiency and mild reaction conditions, but also can be magnetically separated and is easy to recycle, thereby reducing production costs. Detailed Embodiments
[0025] The following describes the detailed embodiments of the present invention in detail, but it should be understood that the protection scope of the present invention is not limited by the detailed embodiments.
[0026] Example 1
[0027] This example provides a production process of diuron. The specific steps include: adding 20 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene, and 0.6 part of Co3O4-SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 2 parts of a 50% aqueous solution of dimethylamine by mass, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and obtaining diuron after centrifugation, washing, and drying.
[0028] The Co3O4-SeO2 / N-MCNTs is prepared by the following steps:
[0029] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate, and 1 part of anhydrous sodium acetate in 60 parts of a 60% ethylene glycol solution by weight, add 0.6 part of nitrogen-doped magnetic carbon nanotubes, soak for 9 h, react at 210 °C for 11 h. After the reaction is completed, wash and dry the sample with absolute ethanol and deionized water to obtain Co3O4-SeO2 / N-MCNTs.
[0030] The nitrogen-doped magnetic carbon nanotubes are prepared through the following steps:
[0031] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic, then add melamine and disperse it by ultrasonic to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. Stir the solution at 70 °C until the ethanol completely evaporates to obtain a precursor. After drying and grinding the precursor, place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep it at this temperature for 2 h for high-temperature calcination pyrolysis to obtain the nitrogen-doped magnetic carbon nanotubes.
[0032] Example 2
[0033] This example provides a production process of diuron. The specific steps include: adding 25 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene, and 0.75 part of Co3O4-SeO2 / N-MCNTs into a reaction kettle by weight for mixing, heating to 23 °C, adding 3 parts of a 50% aqueous solution of dimethylamine, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and then obtaining diuron after centrifugation, washing, and drying.
[0034] The Co3O4-SeO2 / N-MCNTs are prepared through the following steps:
[0035] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate, and 1 part of anhydrous sodium acetate in 60 parts of a 60% ethylene glycol solution by weight, add 0.6 part of nitrogen-doped magnetic carbon nanotubes, soak for 9 h, react at 210 °C for 11 h. After the reaction ends, wash and dry the sample with absolute ethanol and deionized water to obtain Co3O4-SeO2 / N-MCNTs.
[0036] The nitrogen-doped magnetic carbon nanotubes are prepared through the following steps:
[0037] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic, then add melamine and disperse it by ultrasonic to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. Stir the solution at 70 °C until the ethanol completely evaporates to obtain a precursor. After drying and grinding the precursor, place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep it at this temperature for 2 h for high-temperature calcination pyrolysis to obtain the nitrogen-doped magnetic carbon nanotubes.
[0038] Example 3
[0039] This embodiment provides a production process of diuron, and the specific steps include: adding 25 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene and 1 part of Co3O4-SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 3 parts of an aqueous dimethylamine solution with a mass fraction of 50%, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and obtaining diuron after centrifugation, washing and drying;
[0040] The Co3O4-SeO2 / N-MCNTs is prepared by the following steps:
[0041] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate and 1 part of sodium acetate anhydrous in 60 parts of an ethylene glycol solution with a mass fraction of 60% by weight, add 0.6 part of nitrogen-doped magnetic carbon nanotubes and soak for 9 h, then react at 210 °C for 11 h. After the reaction ends, wash and dry the sample with absolute ethanol and deionized water to obtain Co3O4-SeO2 / N-MCNTs.
[0042] The nitrogen-doped magnetic carbon nanotubes are prepared by the following steps:
[0043] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic wave, then add melamine and disperse it by ultrasonic wave to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2; continuously stir the solution at 70 °C until the ethanol completely volatilizes to obtain a precursor; dry and grind the precursor, then place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep warm for 2 h for high-temperature calcination pyrolysis to obtain nitrogen-doped magnetic carbon nanotubes.
[0044] Example 4
[0045] This embodiment provides a production process of diuron, and the specific steps include: adding 25 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene and 1.25 parts of Co3O4-SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 3 parts of an aqueous dimethylamine solution with a mass fraction of 50%, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and obtaining diuron after centrifugation, washing and drying;
[0046] The Co3O4-SeO2 / N-MCNTs is prepared by the following steps:
[0047] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate and 1 part of sodium acetate anhydrous in 60 parts of an ethylene glycol solution with a mass fraction of 60% by weight, add 0.6 part of nitrogen-doped magnetic carbon nanotubes and soak for 9 h, then react at 210 °C for 11 h. After the reaction ends, wash and dry the sample with absolute ethanol and deionized water to obtain Co3O4-SeO2 / N-MCNTs.
[0048] The nitrogen-doped magnetic carbon nanotubes are prepared by the following steps:
[0049] Ferric chloride hexahydrate is dissolved in absolute ethanol by ultrasonic treatment, and then melamine is added and ultrasonically dispersed to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. The solution is continuously stirred at 70 °C until the ethanol is completely evaporated to obtain a precursor. After the precursor is dried and ground, it is placed in a tubular furnace filled with Ar gas, and the furnace temperature is raised to 750 °C at a rate of 3 °C / min and kept at this temperature for 2 h for high-temperature calcination pyrolysis to obtain the nitrogen-doped magnetic carbon nanotubes.
[0050] Example 5
[0051] This example provides a production process of diuron. The specific steps include: adding 25 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene and 1.25 parts of Co3O4-SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 3 parts of a 50% aqueous solution of dimethylamine by mass, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and then obtaining diuron after centrifugation, washing and drying.
[0052] The Co3O4-SeO2 / N-MCNTs are prepared by the following steps:
[0053] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate and 1 part of anhydrous sodium acetate by weight in 60 parts of a 60% ethylene glycol solution by mass. Add 0.8 part of nitrogen-doped magnetic carbon nanotubes and soak for 9 h, then react at 210 °C for 11 h. After the reaction is completed, wash the sample with absolute ethanol and deionized water and dry it to obtain Co3O4-SeO2 / N-MCNTs.
[0054] Example 6
[0055] This example provides a production process of diuron. The specific steps include: adding 25 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene and 1.25 parts of Co3O4-SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 3 parts of a 50% aqueous solution of dimethylamine by mass, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and then obtaining diuron after centrifugation, washing and drying.
[0056] The Co3O4-SeO2 / N-MCNTs are prepared by the following steps:
[0057] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate and 1 part of anhydrous sodium acetate in 60 parts of a 60% by mass ethylene glycol solution by weight. Add 1 part of nitrogen-doped magnetic carbon nanotubes and soak for 9 h, then react at 210 °C for 11 h. After the reaction is completed, wash the sample with absolute ethanol and deionized water and dry it to obtain Co3O4-SeO2 / N-MCNTs.
[0058] The nitrogen-doped magnetic carbon nanotubes are prepared by the following steps:
[0059] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic treatment, then add melamine and disperse it by ultrasonic treatment to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. Stir the solution at 70 °C until the ethanol completely evaporates to obtain a precursor. After drying and grinding the precursor, place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep it at this temperature for 2 h for high-temperature calcination pyrolysis to prepare nitrogen-doped magnetic carbon nanotubes.
[0060] Comparative Example 1
[0061] This comparative example provides a production process of diuron. The specific steps include: add 20 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene and 0.6 part of Co3O4 / N-MCNTs into a reaction kettle by weight for mixing, heat up to 23 °C, add 2 parts of a 50% by mass aqueous dimethylamine solution, heat up to 45 °C for reaction, cool to room temperature, keep warm for 1 h, and then obtain diuron after centrifugation, washing and drying.
[0062] The Co3O4-SeO2 / N-MCNTs are prepared by the following steps:
[0063] Dissolve 10 parts of cobalt chloride hexahydrate and 1 part of anhydrous sodium acetate in 60 parts of a 60% by mass ethylene glycol solution by weight. Add 0.6 part of nitrogen-doped magnetic carbon nanotubes and soak for 9 h, then react at 210 °C for 11 h. After the reaction is completed, wash the sample with absolute ethanol and deionized water and dry it to obtain Co3O4 / N-MCNTs.
[0064] The nitrogen-doped magnetic carbon nanotubes are prepared by the following steps:
[0065] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic treatment, then add melamine and disperse it by ultrasonic treatment to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. Stir the solution at 70 °C until the ethanol completely evaporates to obtain a precursor. After drying and grinding the precursor, place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep it at this temperature for 2 h for high-temperature calcination pyrolysis to prepare nitrogen-doped magnetic carbon nanotubes.
[0066] Comparative Example 2
[0067] This comparative example provides a production process of diuron. The specific steps include: adding 20 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene, and 0.6 part of SeO2 / N-MCNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 2 parts of a 50% aqueous dimethylamine solution, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and obtaining diuron after centrifugation, washing, and drying.
[0068] The Co3O4-SeO2 / N-MCNTs is prepared through the following steps:
[0069] Dissolve 10 parts of selenium nitrate and 1 part of anhydrous sodium acetate by weight in 60 parts of a 60% ethylene glycol solution, add 0.6 part of nitrogen-doped magnetic carbon nanotubes, soak for 9 h, react at 210 °C for 11 h. After the reaction ends, wash and dry the sample with absolute ethanol and deionized water to obtain SeO2 / N-MCNTs.
[0070] The nitrogen-doped magnetic carbon nanotubes are prepared through the following steps:
[0071] Dissolve ferric chloride hexahydrate in absolute ethanol by ultrasonic, then add melamine and disperse ultrasonically to form a solution. The molar ratio of ferric chloride hexahydrate to melamine is 1:2. Stir the solution at 70 °C until the ethanol completely evaporates to obtain a precursor. Dry and grind the precursor, then place it in a tubular furnace filled with Ar gas, raise the furnace temperature to 750 °C at a rate of 3 °C / min, and keep warm for 2 h for high-temperature calcination pyrolysis to obtain nitrogen-doped magnetic carbon nanotubes.
[0072] Comparative Example 3
[0073] This example provides a production process of diuron. The specific steps include: adding 20 parts of 3,4-dichlorophenyl isocyanate, 100 parts of toluene, and 0.6 part of Co3O4-SeO2 / CNTs by weight into a reaction kettle for mixing, heating to 23 °C, adding 2 parts of a 50% aqueous dimethylamine solution, heating to 45 °C for reaction, cooling to room temperature, keeping warm for 1 h, and obtaining diuron after centrifugation, washing, and drying.
[0074] The Co3O4-SeO2 / N-MCNTs is prepared through the following steps:
[0075] Dissolve 5 parts of cobalt chloride hexahydrate, 5 parts of selenium nitrate, and 1 part of anhydrous sodium acetate by weight in 60 parts of a 60% ethylene glycol solution, add 0.6 part of carbon nanotubes, soak for 9 h, react at 210 °C for 11 h. After the reaction ends, wash and dry the sample with absolute ethanol and deionized water to obtain Co3O4-SeO2 / N-MCNTs.
[0076] The yield and purity of diuron obtained in Examples 1 - 6 and Comparative Examples 1 - 3 were tested, and the test results are shown in Table 1.
[0077] Table 1
[0078]
[0079]
[0080] As can be seen from Table 1, Examples 1 - 6 had good yields, and the purity of the obtained diuron was also relatively high. By comparing Examples 2, 3, and 4, it can be concluded that increasing the dosage of the catalyst can improve the yield and the purity of diuron; by comparing Examples 4, 5, and 6, it can be obtained that increasing the proportion of nitrogen-doped magnetic carbon nanotubes in the catalyst Co3O4 - SeO2 / N-MCNTs helps to improve the catalytic efficiency, and thus improve the yield and the purity of diuron.
[0081] Compared with Example 1, in Comparative Example 1, Co3O4 - SeO2 / N-MCNTs was replaced with Co3O4 / N-MCNTs, and the yield and the purity of diuron decreased; compared with Example 1, in Comparative Example 2, Co3O4 - SeO2 / N-MCNTs was replaced with SeO2 / N-MCNTs, and the yield and the purity of diuron also decreased; compared with Example 1, in Comparative Example 3, the carrier used was ordinary carbon nanotubes, and Co3O4 - SeO2 / N-MCNTs was replaced with Co3O4 - SeO2 / CNTs, and the yield and the purity of diuron also decreased. The reason is that there is a coordination effect between the nitrogen-doped magnetic carbon nanotubes and Co ions, and Co3O4 and SeO2 have a synergistic effect. Therefore, Co3O4 and SeO2 can be anchored on the nitrogen-doped magnetic carbon nanotubes, making Co3O4 and SeO2 not easily fall off or break during the catalytic process; in addition, the nitrogen-doped magnetic carbon nanotubes have a high specific surface area, which can dynamically adsorb water molecules in the reaction process, effectively avoiding the occurrence of side reactions where 3,4-dichlorophenyl isocyanate hydrolyzes to form N,N-bis(3,4-dichlorophenyl)urea; therefore, Co3O4 - SeO2 / N-MCNTs has rich active sites, good chemical stability, and can avoid the occurrence of side reactions, thereby improving the yield and purity of diuron.
[0082] The above only discloses several specific embodiments of the present invention. However, the embodiments of the present invention are not limited thereto, and any changes that can be thought of by those skilled in the art should fall within the protection scope of the present invention.
Claims
1. A production process of diuron, characterized in that, The specific steps include: adding 3,4-dichlorophenyl isocyanate, toluene and a catalyst into a reaction kettle for mixing, heating to 22 - 24 °C, adding an aqueous solution of dimethylamine, heating to 40 - 50 °C for reaction, cooling to room temperature, keeping warm for 0.5 - 1 h, and then obtaining diuron after centrifugation, washing and drying. The catalyst is cobalt selenide oxide supported on nitrogen-doped magnetic carbon nanotubes, denoted as Co3O4 - SeO2 / N - MCNTs.
2. The production process of diuron according to claim 1, characterized in that, The weight part ratio of the amounts of 3,4-dichlorophenyl isocyanate, toluene and the aqueous solution of dimethylamine is 20 - 25:100:2 - 3.
3. The production process of diuron according to claim 1, characterized in that, The amount of the catalyst used is 3 - 5% of the mass of 3,4-dichlorophenyl isocyanate.
4. The production process of diuron according to claim 1, characterized in that, The mass fraction of the aqueous solution of dimethylamine is 50 - 55%.
5. The production process of diuron according to claim 1, characterized in that, The catalyst Co3O4 - SeO2 / N - MCNTs is prepared by the following steps: Dissolving cobalt chloride hexahydrate, selenium nitrate and sodium acetate anhydride in an ethylene glycol solution, adding nitrogen-doped magnetic carbon nanotubes and soaking for 8 - 10 h, then reacting at 200 - 220 °C for 10 - 12 h. After the reaction ends, washing and drying the sample with absolute ethanol and deionized water to obtain Co3O4 - SeO2 / N - MCNTs.
6. The production process of diuron according to claim 5, characterized in that, The weight part ratio of the amounts of cobalt chloride hexahydrate, selenium nitrate, sodium acetate anhydride, nitrogen-doped magnetic carbon nanotubes and the ethylene glycol solution is 5:5:1:0.6 - 1:
60.
7. The production process of diuron according to claim 5, characterized in that, The mass fraction of the ethylene glycol solution is 60 - 70%.
8. The production process of diuron according to claim 5, characterized in that, The nitrogen-doped magnetic carbon nanotubes are prepared by the following steps: Dissolving ferric chloride hexahydrate in absolute ethanol by ultrasonic wave, then adding melamine and dispersing by ultrasonic wave to form a solution; continuously stirring the solution at 70 - 75 °C until the ethanol completely volatilizes to obtain a precursor; drying and grinding the precursor, and then placing it in a tubular furnace filled with Ar gas and carrying out high-temperature calcination pyrolysis according to the set heating program to prepare the nitrogen-doped magnetic carbon nanotubes.
9. The production process of diuron according to claim 8, characterized in that, The molar ratio of ferric chloride hexahydrate to melamine is 1∶2.
10. The production process of diuron according to claim 8, characterized in that, The set heating program is: raising the furnace temperature to 650 - 850 °C at a rate of 3 °C / min and keeping warm for 2 h.