Preparation method of walnut shell-based hierarchical porous carbon with high capacitive properties
A technology of hierarchical porous and walnut shells, applied in chemical instruments and methods, hybrid capacitor electrodes, carbon compounds, etc., can solve problems such as waste of resources
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Embodiment 1
[0024] Example 1 (without microwave-assisted activation)
[0025] (1) Soak lye treatment Weigh fully dried walnut shell powder 2.0g and 4.0g KOH (guaranteed mass ratio, pretreatment powder: KOH=1:1-3), add 25mL of distilled water (guaranteed solid-liquid mass volume ratio of 1 : 4~10), stir evenly, soak for 6-12h, transfer to an oven at 80-100 ℃ and dry into a solid. Then pulverize with a pulverizer to obtain powdery walnut shell powder, which is sieved through a 60-mesh sieve to obtain walnut shell powder (with a particle size of about 200 μm).
[0026] (2) One-step carbonization treatment Take 2.0~3.0g of potassium hydroxide and walnut shell powder mixture into the tube furnace, N 2 under protection, at 3-5°C min -1 The heating rate was raised to about 300 °C, maintained for 0.5 h, and then continued to heat up to 800 °C for another 2 h to fully carbonize and activate.
[0027] (3) Carbide post-treatment After natural cooling, take out the carbonized product, wash with 0....
Embodiment 2
[0031] Example 2 (microwave power is 320W)
[0032] (1) Pulverization Soak the walnut shells in distilled water to remove surface impurities, then place them in an oven at 60°C to dry to constant weight, and then pulverize them with a pulverizer to obtain powdered walnut shell powder, which is passed through a 60-mesh sieve to obtain walnut shells powder;
[0033] (2) Microwave preactivation Weigh 5.0g of walnut shell powder into a conical flask, then add 50mL of dilute hydrochloric acid solution (2mol / L), stir for 0.5h~1h, and then transfer it to a microwave oven with a microwave power of 320W Heat treatment for 10-15min under the same conditions to obtain a dark brown paste. After natural cooling, suction filtration is performed, repeatedly washed with distilled water until neutral, and dried in an oven at 80-100°C for 12h to obtain pretreated walnut shell powder.
[0034] (3) Dry and weigh 2.0g of pretreated walnut shell powder and 4.0g of KOH (guaranteed mass ratio, pretr...
Embodiment 3
[0040] Embodiment 3 (microwave power is 480W)
[0041] (1) The preparation method of walnut shell powder is the same as step (1) in Example 2;
[0042] (2) Microwave pre-activation Weigh 5.0g of walnut powder into a conical flask, then add 50mL of dilute hydrochloric acid solution (2mol / L), stir for 0.5h~1h, and then transfer it to a microwave oven with a microwave power of 480W. Heat treatment under conditions for 10-15min to obtain a dark brown paste. After natural cooling, suction filtration is carried out, repeatedly washed with distilled water until neutral, and dried in an oven at 80-100°C for 12h.
[0043] Steps (3)-(7) are as described in Example 2.
[0044] (8) Product test results figure 2 The results of the infrared spectrum analysis showed that the hydroxyl peak and carbonyl peak of the microwave power pretreated at 480W were lower than those of the blank sample and 320W treatment, indicating that the chemical bonds were destroyed to a great extent during the mi...
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