Method for extracting lignin from biomass by liquid nitrogen coupled microwave pretreatment
A pretreatment and lignin technology, which is applied in fiber raw material treatment, bulk chemical production, textile and paper making, etc., can solve problems such as recycling problems cannot be effectively solved, continuous production cannot be achieved, acid-base ammonia gas consumption, etc. , to achieve the effects of increased yield, less damage, and reduced input
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Embodiment 1
[0022] Sawdust (birch) is crushed and passed through a 20-mesh sieve, and 100g is taken as a raw material for low-temperature pretreatment with liquid nitrogen; dried and immersed in liquid nitrogen, the immersion time is 2min, and the number of immersion times is 5 times, and then the water content of the material is adjusted to 25wt%. , mix the raw materials evenly, and let it stand for 1h, put it into a microwave device for processing, the microwave power is 2kW, the processing time is 100s, repeat the microwave processing twice, and then carry out the determination of water content and X-ray diffraction to determine the degree of crystallinity; the end of microwave processing After that, put it into a 200ml reaction kettle, use 30% concentration (volume concentration) of 1,4-butanediol to extract, the solid-liquid ratio is 1:6 (g / mL), and the extraction temperature is 160°C. The extraction time was 120 min, filtered under reduced pressure, the supernatant was adjusted to pH...
Embodiment 2
[0025] Corn stalks are crushed and passed through a 30-mesh sieve, and 100g is taken as a raw material for low-temperature pretreatment with liquid nitrogen; dried and immersed in liquid nitrogen for 5 minutes and 3 times of immersion, and then adjust the water content of the material to 35wt%, uniform Mix the raw materials and let stand for 3 hours, put them into a microwave device for processing, the microwave power is 5kW, the processing time is 200s, repeat the microwave treatment twice, then carry out the determination of water content and X-ray diffraction to determine the degree of crystallinity; after the microwave treatment is completed, Put it into a 200ml reaction kettle, use 30% concentration (volume concentration) of 1,4-butanediol for leaching, the solid-liquid ratio is 1:6 (g / mL), the leaching temperature is 180°C, and the leaching time After 180 min, filter under reduced pressure, adjust the pH to 4 with 2 mol / L hydrochloric acid in the supernatant and centrifug...
Embodiment 3
[0028] Walnut shells are crushed and passed through a 20-mesh sieve, and 100g is taken as a raw material for liquid nitrogen low-temperature pretreatment; dried and immersed in liquid nitrogen, the immersion time is 12min, and the number of immersion times is 8 times, and then the water content of the sample is adjusted to 40wt%. Mix the raw materials and let them stand for 4 hours, put them into a microwave device for processing, the microwave power is 8kW, the processing time is 300s, repeat the microwave treatment 3 times, then carry out the determination of water content and the determination of crystallinity by X-ray diffraction; after microwave treatment, use Choline chloride / boric acid (3:5) combined deep eutectic solvent (DES) for leaching, the solid-to-liquid ratio is 1:12 (g / mL), leaching at 90°C for 120min; filter under reduced pressure, The supernatant was centrifuged when the pH was adjusted to 4 with 2 mol / L hydrochloric acid, and the obtained sediment was dried t...
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