Method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin
A technology for lignin and vanillin, which is applied in the field of catalytic oxygenolysis of lignin to prepare extracts containing vanillin and syringaldehyde, can solve the problems of harsh reaction conditions of strong acid and strong alkali, low yield of target products, corrosive environment of equipment and the like, Achieve the effect of low price, stable hydrothermal performance and easy oxidative depolymerization
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example 1
[0045] Example 1: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 , CeCuO 3 , CeFeO 3 , CeNiO 3 One of them is placed in a reaction kettle, and 20ml of ethanol / water mixed solvent is added, and the volume ratio of ethanol and water in the mixed solvent is 1:1; the reaction kettle is filled with nitrogen to 1MPa, and then exhausted, and repeated three times Complete the purging process; then feed oxygen into the reactor to 0.6MPa; set the reaction temperature to 180°C and the reaction time to 60 minutes. After the reaction is over, place the reactor in an ice-water mixture to cool to normal temperature and discharge, filter Oxidation residue was obtained; the obtained filtrate was rotary evaporated until the solvent was evaporated to dryness, and ethyl acetate was added for extraction, and the organic phase was combined and fixed to 10ml for GC-MS detection; 3 When used as a catalyst, the yields of vanillin and syringaldehyde in the extract all reached th...
example 2
[0046] Example 2: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 Placed in the reaction kettle, the volume ratio of ethanol and water in the mixed solvent is 1:1; fill the reaction kettle with nitrogen to 1MPa, then exhaust, repeat three times to complete the purging process; then pass into the reaction kettle Oxygen to 0.6MPa; set the reaction temperature to 120°C, and the reaction time to 60min; after the reaction, place the reaction kettle in an ice-water mixture to cool to room temperature and discharge the material, and filter to obtain the oxidation residue; the obtained filtrate is rotary evaporated until the solvent is evaporated to dryness, and added Extract with ethyl acetate, combine the organic phases and settle to 10ml, and carry out GC-MS detection; at this moment, vanillin and syringaldehyde are not detected in the extract, as image 3 , 4 shown.
example 3
[0047] Example 3: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 Put it in the reaction kettle, add 20ml of ethanol / water mixed solvent, the volume ratio of ethanol and water in the mixed solvent is 1:1; fill the reaction kettle with nitrogen to 1MPa, then exhaust, repeat three times to complete the purging process ; Immediately after, feed oxygen into the reactor to 0.6MPa; set the reaction temperature to 150°C and the reaction time to 60min, place the reactor in an ice-water mixture to cool to normal temperature and discharge the material after the reaction, and filter to obtain the oxidation residue; The filtrate was rotary evaporated until the solvent was evaporated to dryness, and ethyl acetate was added for extraction, the organic phases were combined and fixed to 10ml, and then detected by GC-MS; the yields of vanillin and syringaldehyde in the extract were 0.8%, 0.4% respectively. %,Such as image 3 , 4 shown.
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