Method used for extracting lignin from lignocelluloses raw material and preparing p-hydroxy benzaldehyde via catalytic conversion
A technology of p-hydroxybenzaldehyde and lignocellulose, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as easy repolymerization and complexation reactions, complex structures, etc. Low, high catalytic activity, high activity effect
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Embodiment 1
[0021] Take corn stover as raw material, use 40% 1,4-butanediol aqueous solution as solvent, solid-to-liquid ratio 1:4, temperature 220°C, cool after 2h reaction, filter, and weigh the filter cake; add three times the volume of the filtrate Deionized water is allowed to stand overnight and filtered, and the obtained filter residue is washed and vacuum dried to obtain corn stover to extract lignin. The lignin is used in the catalytic conversion system, the reaction conditions: lignin concentration 20g / L, LaFe 0.2 Cu 0.8 O 3 Concentration 2g / L, use NaOH solution to adjust the pH value of the system to 13, temperature 160℃, charge O 2 Pressure 8bar, reaction for 2h, take it out and centrifuge to get the catalyst, the supernatant is adjusted to pH 1-2 with concentrated HCl, and unreacted lignin is precipitated; filtered, lignin washed and weighed, the volume of the filtrate is recorded, sampled, and analyzed by HPLC The yield of p-hydroxybenzaldehyde was 3.06%.
Embodiment 2
[0023] Using walnut shell as raw material, 60% 1,4-butanediol aqueous solution is used as solvent, solid-liquid ratio is 1:8, temperature is 180℃, after 2.5 hours of reaction, cooled, filtered, and the filter cake is recovered and weighed; the filtrate is added to three times the volume The deionized water is allowed to stand overnight and filtered. The obtained filter residue is washed and vacuum dried to obtain lignin from walnut shells. The lignin is used in the catalytic conversion system, the reaction conditions: lignin concentration 2g / L, LaNi 0.2 Cu 0.8 O 3 Concentration 2g / L, adjust the pH value of the system to 11 with NaOH solution, temperature 180℃, charge O 2 Pressure 2bar, reaction for 2h, take it out and centrifuge to obtain the catalyst, the supernatant is adjusted to pH 1-2 with concentrated HCl, and unreacted lignin is precipitated; filtered, lignin washed and weighed, the volume of the filtrate is recorded, sampled, and analyzed by HPLC The yield of p-hydroxybe...
Embodiment 3
[0025] Using coconut shell as raw material, using 80% 1,4-butanediol aqueous solution as solvent, solid-liquid ratio 1:10, temperature 200℃, cooling after 4h reaction, filtering, filter cake recovery and weighing; adding three times the volume of the filtrate Deionized water is allowed to stand overnight and filtered, and the obtained filter residue is washed and vacuum dried to obtain lignin from walnut shells. The lignin was used in the catalytic conversion system, the reaction conditions: lignin concentration 10g / L, 5% loading The molecular sieve concentration is 1g / L, the pH value of the system is adjusted to 9 with NaOH solution, the temperature is 140℃, and O is charged 2 The pressure is 6bar, the reaction is 1.5h, and the catalyst is obtained by centrifugation after removal. The supernatant is adjusted to pH 1-2 with concentrated HCl to precipitate unreacted lignin; filtered, washed with lignin and weighed, the volume of the filtrate is recorded, sampled, and analyzed by ...
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