Method for grafting polycaprolactone onto hemicellulose in polar aprotic solvent system
A polar aprotic and hemicellulose technology, which is applied in the field of high-value utilization of biomass, can solve the problems of variable structure, solubility and reactivity changes, complex hemicellulose composition, etc., and achieve strong solubility and improved The effect of processability
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[0023] Example 1:
[0024] The hemicellulose-grafted polycaprolactone of this embodiment is in DMSO / LiCl, and its specific process is as follows:
[0025] Step 1. Hemicellulose (xylan content 85%) was vacuum dried at 50°C for 12h; hemicellulose was dispersed in DMSO / LiCl (LiCl mass percentage 6%), stirred at 80°C under nitrogen protection 2h, a hemicellulose solution was obtained;
[0026] Step 2. Slowly add caprolactone monomer dropwise at a ratio of caprolactone monomer to hemicellulose mass ratio of 18:1, and react at 100°C for 24h;
[0027] Step 3. After the reaction solution was cooled to room temperature, add ethanol to precipitate (150ml*3 times), filter and add 150ml of dichloromethane to the precipitate, stir magnetically for 72h, filter, and dry under reduced pressure at 50°C and vacuum of 0.1MPa for 48h , that is, the final product hemicellulose-grafted polycaprolactone is obtained.
[0028] Infrared and hydrogen spectra of unmodified hemicellulose and hemicellul...
Example Embodiment
[0035] Example 2:
[0036] The hemicellulose-grafted polycaprolactone of this embodiment is in DMAc / LiCl, and its specific process is as follows:
[0037] Step 1. Hemicellulose (xylan content 55%) was vacuum dried at 50°C for 12h; hemicellulose was dispersed in DMAc / LiCl (LiCl mass percentage 0.1%), stirred at 150°C under nitrogen protection 24h, a hemicellulose solution was obtained;
[0038] Step 2. Slowly add caprolactone monomer dropwise at a ratio of caprolactone monomer to hemicellulose mass ratio of 52:1, and react at 30°C for 0.5h;
[0039] Step 3. After the reaction solution is cooled to room temperature, add ethanol precipitation (150ml*3 times), filter and add 150ml dichloromethane to the precipitation, stir magnetically for 72h, filter, freeze-dry at -40°C for 36h to obtain the final product Hemicellulose grafted polycaprolactone. The infrared spectra of the prepared hemicellulose-grafted polycaprolactone were compared with figure 1 Similar to the hydrogen spec...
Example Embodiment
[0040] Example 3:
[0041] The hemicellulose-grafted polycaprolactone of this embodiment is in DMF / LiCl, and its specific process is as follows:
[0042] Step 1. Hemicellulose (xylan content 65%) was vacuum dried at 50°C for 12h; hemicellulose was dispersed in DMF / LiCl (LiCl mass percentage 15%), stirred at 30°C under nitrogen protection 0.1h to obtain hemicellulose solution;
[0043] Step 2. Slowly add caprolactone monomer dropwise at a ratio of caprolactone monomer to hemicellulose mass ratio of 0.5:1, and react at 150°C for 16h;
[0044] Step 3. After the reaction solution is cooled to room temperature, add ethanol to precipitate (150ml*3 times), filter and add 150ml of dichloromethane to the precipitate, stir magnetically for 72h, filter, and dry under reduced pressure at 20°C and a vacuum of 0.1MPa for 48h , that is, the final product hemicellulose-grafted polycaprolactone is obtained.
[0045] The infrared spectra of the prepared hemicellulose-grafted polycaprolactone w...
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