Oxygen-doped surface modification silkworm excrement based hierarchical pore carbon material and preparation method and application thereof
A surface modification and multi-level pore technology, applied in the field of carbon materials, can solve problems such as pollution, low pesticide utilization efficiency, and excessive pesticide residues in agricultural products, and achieve the effect of increasing porosity, specific surface area, and high adsorption capacity
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Embodiment 1
[0034] A preparation method of O-doped surface-modified silkworm excrement-based hierarchical porous carbon material, comprising the following steps,
[0035] (1) The original silkworm excrement and the ZnCl of mass concentration 0.25g / mL 2 The solution was mixed and swollen at 30°C according to the plastid ratio of 1:100 for 3.0h, then the silkworm excrement was fished out, and the silkworm excrement was freeze-dried, first frozen at -20°C for 4h, and then cooled to -60°C for freezing. Dry for 24 hours to obtain freeze-dried silkworm excrement.
[0036] (2) freeze-dried silkworm excrement in N 2 In the atmosphere, the temperature was raised to 300°C at a rate of 5°C / min, and kept at 300°C for 5.0h to carry out the pore expansion reaction. After naturally cooling down to room temperature, the obtained solid was dissolved in 1mol / L HCl to wash and dissolve ZnCl 2 , and then washed with deionized water to pH ≈ 7, then centrifuged, placed in an oven to dry overnight, and obtain...
Embodiment 2
[0039] (1) The original silkworm excrement and the ZnCl of mass concentration 0.25g / mL 2 The solution was mixed and swollen at 35°C according to the plastid ratio of 1:120 for 2.5 hours, and then the silkworm excrement was fished out, and the silkworm excrement was freeze-dried. It was first frozen at -20°C for 3 hours, and then cooled to -55°C. Dry for 36 hours to obtain freeze-dried silkworm excrement.
[0040] (2) Raise the freeze-dried silkworm excrement to 350°C at a heating rate of 5°C / min in an Ar atmosphere, and keep it at 350°C for 4.0h to carry out the pore expansion reaction. After naturally cooling down to room temperature, dissolve the obtained solid Wash and dissolve ZnCl in 1mol / L HCl 2 , and then washed with deionized water to pH ≈ 7, then centrifuged, placed in an oven to dry overnight, and obtained the silkworm excrement-based hierarchical porous carbon material after drying.
[0041] (3) Put 1.0g silkworm excrement-based hierarchical porous carbon material...
Embodiment 3
[0043] (1) The original silkworm excrement and the ZnCl of mass concentration 0.30g / mL 2 The solution was mixed and swollen at 40°C according to the plastid ratio of 1:140 for 2.0h, and then the silkworm excrement was fished out, and the silkworm excrement was freeze-dried, firstly frozen at -25°C for 2h, and then cooled to -50°C for freezing. Dry for 48 hours to obtain freeze-dried silkworm excrement.
[0044] (2) freeze-dried silkworm excrement in N 2 In the atmosphere, the temperature was raised to 400°C at a rate of 5°C / min, and kept at 400°C for 3.0h to carry out the pore expansion reaction. After the natural temperature dropped to room temperature, the obtained solid was dissolved in 1mol / L HCl to wash and dissolve ZnCl 2 , and then washed with deionized water to pH ≈ 7, then centrifuged, placed in an oven to dry overnight, and obtained the silkworm excrement-based hierarchical porous carbon material after drying.
[0045] (3) Put 1.0g silkworm excrement-based hierarch...
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