Supercritical liquefaction method for biomass
A biomass and bio-oil technology, which is applied in the preparation of biological raw materials, liquid hydrocarbon mixtures, petroleum industry, etc., can solve the problems of limiting the utilization of biomass pyrolysis oil, and achieve the effect of mild liquefaction process conditions
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Embodiment 1
[0015] 10g hardwood sawdust, 6g sodium hydroxide and sodium sulfide mixed alkali catalyst (sodium sulfide content is 12.5%), 95% (v / v) ethanol of 100ml add autoclave, replace the air in the still with nitrogen after sealing, and Pour into nitrogen 2MPa, heat up to 285°C, pressurize to 12.5MPa, keep in this state for 10 minutes, feed cooling water in the cooling coil in the autoclave to cool the material to room temperature, take out the material, and use 150ml of 50% ( v / v) ethanol solution to clean the autoclave, the washing liquid is incorporated into the reaction mass, and the pH is adjusted to pH 1-3 with 2mol / L hydrochloric acid, and left standing overnight. Filter the material, extract the filtrate with 4×50ml of dichloromethane, then use a rotary evaporator to remove the dichloromethane at 40°C, and remove the water and ethanol inside under reduced pressure at the same temperature to obtain liquefied oil A5.03g. The filter residue was extracted with dichloromethane unt...
Embodiment 2
[0017] Add 10g of wood hydrolysis residue, 6g of sodium hydroxide, and 100ml of 95% (v / v) ethanol into the autoclave, replace the air in the autoclave with nitrogen after sealing, and flush into nitrogen at 2MPa, heat up to 290°C, and pressurize to 12.6MPa, after maintaining this state for 10min, feed cooling water into the cooling coil in the autoclave to cool the material to room temperature, take out the material, clean the autoclave with 150ml of 50% (v / v) ethanol solution, wash the liquid and Add the reaction materials, adjust the pH to pH 1-3 with 2mol / L hydrochloric acid, and let stand overnight. Filter the material, extract the filtrate with 4×50ml of dichloromethane, then use a rotary evaporator to remove the dichloromethane at 40°C, and remove the water and ethanol inside under reduced pressure at the same temperature to obtain liquefied oil A4.80g. The filter residue was extracted with dichloromethane until the extract was colorless, and the dichloromethane was rem...
Embodiment 3
[0019] Add 80% (v / v) methyl alcohol of 10g woody biomass hydrolysis residue, 4g sodium hydroxide, 100ml to autoclave, replace the air in the still with nitrogen after sealing, and flush into nitrogen 2MPa, heat up to 285 ℃, add Press down to 12.MPa, keep in this state for 10 minutes, feed cooling water into the cooling coil in the autoclave to cool the material to room temperature, take out the material, and clean the autoclave with 150ml of 50% (v / v) methanol solution , and the washing liquid is incorporated into the reaction material, and the pH is adjusted to a pH value of 1-3 with 2 mol / l hydrochloric acid, and left to stand overnight. Filter the material, extract the filtrate with 4×50ml of dichloromethane, then use a rotary evaporator to remove the dichloromethane at 40°C, and remove the water and ethanol inside under reduced pressure at the same temperature to obtain liquefied oil A3.12g. The filter residue was extracted with dichloromethane until the extract was color...
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