Method for preparing Ni-loaded mesoporous carbon materials through solid-state synthesis method
A solid-state synthesis, mesoporous carbon technology, applied in the field of mesoporous carbon materials, can solve the problems of small pore size, difficult to widely use, and difficult to apply biomass catalytic depolymerization, etc., to achieve the effect of large pore size
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Embodiment 1-4
[0027] Weigh 1g of tannin and 0.8g of F127 (polyoxyethylene-polyoxypropylene-polyoxyethylene, Sigma-Aldrich, P2443), and add 6, 12, 18, 24 stainless steel balls into the In the ball mill tank, ball mill for 0.5h, then weigh 3mmol of nickel acetate tetrahydrate and add it, continue ball milling for 0.5h, use deionized water and ethanol to wash three times, and dry at room temperature overnight. 2 Atmosphere, calcined at 450°C for 2h to obtain Ni / MC, Ni / MC 12 , Ni / MC 18 , Ni / MC 24 catalyst.
[0028] The eucalyptus wood powder that takes 2g, the corresponding catalyst in the table 1 of 0.2g and the ethanol of 50ml will be put in the autoclave, utilize hydrogen to replace gas repeatedly 4 times, fill into 2MPa H 2 , 280 ℃ for 6h, after the end of the reaction, quickly use a water bath to drop the reactor to room temperature. The gas was collected, the product was separated, and the yield of the obtained phenolic monomers was shown in Table 1.
[0029] The adsorption-desorptio...
Embodiment 5
[0032] Embodiment 5,6:
[0033] Weigh 1g of tannin and add 0.6g and 1g of F127 respectively according to Table 2, and add them into the ball mill jar together with 6 stainless steel balls, mill for 0.5h, then weigh 3mmol of nickel acetate tetrahydrate and add it, continue ball milling After 0.5h, use deionized water and ethanol to wash several times and then dry overnight at room temperature. 2 atmosphere, calcination at 450°C for 2h to obtain Ni / MC 0.6 , Ni / MC 1 catalyst. Weigh 2g of eucalyptus powder, 0.2g of catalyst and 50ml of ethanol into the autoclave, use hydrogen to replace the gas repeatedly 4 times, and fill with 2MPa H 2 , 280 ℃ for 6h, after the end of the reaction, quickly use a water bath to drop the reactor to room temperature. The gas was collected, the product was separated, and the yield of phenolic monomers obtained was shown in Table 2.
[0034] Table 2 Effect of raw material ratio of catalyst on hydrogenolysis of eucalyptus powder
[0035]
Embodiment 7-9
[0037] Weigh 1g of alkali lignin (AL), dealkalized lignin (DL) and organic solvent lignin (OL) according to the carbon source described in Table 3, and weigh 0.8g of F127, and mix with 6 stainless steel Add the balls together into the ball mill jar, mill for 0.5h, then weigh 3mmol of nickel acetate tetrahydrate and add it, continue the ball milling for 0.5h, wash with deionized water and ethanol several times, and dry at room temperature overnight, the obtained compound is in the tube N in the furnace 2 atmosphere, calcination at 450°C for 2h to obtain Ni / MC AL , Ni / MC DL , Ni / MC OL catalyst. Weigh 2g of eucalyptus powder, 0.2g of catalyst and 50ml of ethanol into the autoclave, use hydrogen to replace the gas repeatedly 4 times, and fill with 2MPa H 2, 280 ℃ for 6h, after the end of the reaction, quickly use a water bath to drop the reactor to room temperature. The gas was collected, the products were separated, and the yields of the obtained phenolic monomers were shown...
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