Composite material with carbon layer loaded on surface of inorganic carrier and preparation method of composite material

[0036] Example 1

[0037] The composite material of rod-shaped molecular sieve SBA-15 surface coated with carbon layer is prepared, and the preparation steps are as follows:

[0038] Weigh 4g SBA-15 (the specific surface area is 613.56m 2 /g, the average pore diameter is 7.74nm) was put into an oven and dried at 120°C for 12 hours, placed in a 100mL glass flask filled with 40mL of anhydrous toluene under a nitrogen atmosphere, stirred evenly by magnetic force, and added 4.8mL of 3-aminopropyl Trimethoxysilane, stirred and refluxed at 110°C for 12 hours, filtered under reduced pressure and washed with anhydrous toluene, dichloromethane, methanol, water, methanol in sequence, and dried at 80°C to constant weight to obtain the aminated mesoporous support . Put the above-mentioned aminated mesoporous carrier in a 500 mL hydrothermal kettle lined with polytetrafluoroethylene, add 12g of glucose and 200mL of water in sequence, stir evenly, tighten the reaction kettle, and place it in a heating device at 190°C for 5 hours reaction , the reaction system was cooled to room temperature, filtered under reduced pressure and washed with water and methanol until the effluent was colorless, and the solid product was dried at 80°C to constant weight to obtain a hydrothermal carbon-coated mesoporous carrier. Put the above-mentioned hydrothermal carbon layer-coated mesoporous carrier into a quartz boat, place it in a tube furnace with argon gas, heat it from room temperature to 800 °C at 3 °C/min, and bake it for 3 hours. After the reaction is completed, wait to cool to room temperature to collect the material The composite material I (the specific surface area is 326.16m 2 /g, the average pore diameter is 5.49nm, and the carbon layer thickness is 1.13nm). The morphology of the prepared material is as figure 1 As shown, both SBA-15 after carbon coating and the carbon after dissolving SBA-15 still maintain an ordered mesoporous structure, indicating that the carbon layer can be evenly coated on the mesoporous surface of the carrier. figure 2 The nitrogen adsorption and desorption isotherms and pore size distribution diagrams of the products at each stage of the preparation process are provided, which also proves the uniform coating of the carbon layer. At the same time, the specific surface area of ​​the material directly coated with the carbon layer by SBA-15 without modifying the amino group is 431.68m 2/g, the average pore size is 7.69nm, and the pore size distribution is not uniform, indicating that the electrostatic induction of amino groups plays an important role in the preparation process.

[0039] Example 2

[0040] The composite material of rod-shaped molecular sieve SBA-15 surface coated with carbon layer is prepared, and the preparation steps are as follows:

[0041] Weigh 4g SBA-15 (the specific surface area is 613.56m 2 /g, the average pore diameter is 7.74nm) put it in an oven and dry at 100°C for 1 hour, place it in a 100mL glass flask filled with 10mL anhydrous toluene under nitrogen atmosphere, stir it evenly with magnetic force, add 0.4mL 3-aminopropyl Triethoxysilane, stirred and refluxed at 80°C for 12 hours, filtered under reduced pressure and washed with anhydrous toluene, dichloromethane, methanol, water, methanol in sequence, and dried at 60°C to constant weight to obtain aminated mesoporous carrier. Put the above-mentioned aminated mesoporous carrier in a 500mL hydrothermal kettle lined with polytetrafluoroethylene, add 2g of glucose and 20mL of water in sequence, stir evenly, tighten the reaction kettle, and place it in a heating device at 140°C for 2 hours. The reaction system was cooled to room temperature, filtered under reduced pressure and washed with water and methanol until the effluent was colorless, and the solid product was dried at 60°C to constant weight to obtain a hydrothermal carbon-coated mesoporous support. Put the above-mentioned hydrothermal carbon layer-coated mesoporous carrier into a quartz boat, place it in a tube furnace with nitrogen gas, heat it at 1°C/min to 600°C, and roast it for 1 hour. After the reaction is completed, wait for cooling to room temperature to collect the material. Composite material II (specific surface area is 504.22m 2 /g, the average pore diameter is 7.02nm, and the carbon layer thickness is 0.36nm).

[0042] Example 3

[0043] The composite material of rod-shaped molecular sieve SBA-15 surface coated with carbon layer is prepared, and the preparation steps are as follows:

[0044] Weigh 4g SBA-15 (the specific surface area is 613.56m 2 /g, the average pore diameter is 7.74nm) put it in an oven and dry at 160°C for 12 hours, place it in a 250mL glass flask filled with 80mL of anhydrous toluene under a nitrogen atmosphere, stir it evenly by magnetic force, add 20mL N-(β-ammonia Ethyl-γ-aminopropyl)methyldimethoxysilane, stirred and refluxed at 120°C for 12 hours, filtered under reduced pressure and washed successively with anhydrous toluene, dichloromethane, methanol, water, methanol, and dried at 150°C The aminated mesoporous carrier can be obtained under the condition of constant weight. Place the above-mentioned aminated mesoporous carrier in a 500mL hydrothermal kettle lined with polytetrafluoroethylene, add 40g of glucose and 200mL of water in sequence, stir evenly, tighten the reaction kettle, and place it in a heating device at 250°C for 5 hours. The reaction system was cooled to room temperature, filtered under reduced pressure and washed with water and methanol until the effluent was colorless, and the solid product was dried at 150 °C to constant weight to obtain a hydrothermal carbon-coated mesoporous support. Put the above-mentioned hydrothermal carbon layer-coated mesoporous carrier into a quartz boat, place it in a tube furnace with argon gas, heat it to 1000°C at 10°C/min, and bake it for 5 hours. Composite material III (the specific surface area is 456.23m 2 /g, the average pore diameter is 2.50nm, and the carbon layer thickness is 2.62nm).