Method for preparing novel sulfonated lignin
A technology of sulfonated lignin and lignin, which is applied in the field of preparation of new sulfonated lignin, can solve the problems of environmental pollution, excessive energy consumption, and low cost, and achieve the effects of wide sources, simple process, and energy saving
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Embodiment 1
[0016] (1) Take 200g of polycondensation enzymatically hydrolyzed lignin, dry it to constant weight, put it into a pulverizer and pulverize it, and screen to obtain lignin of a certain size;
[0017] (2) Add 3 g of lignin to 100 g of water and stir, raise the temperature to 50° C., add 6 g of potassium persulfate compound salt, adjust the pH to 3, add 0.15 g of CuO to initiate the reaction, and keep warm for 1 h.
[0018] (3) Raise the temperature to 70° C., adjust the pH of the reaction solution to 8 with 10 wt % NaOH solution, add 1.5 g of 20% formaldehyde solution by mass fraction, and react for 1 h.
[0019] (4) Heat up to 80°C, add 3g of sodium sulfite, and react for 3h. After cooling to room temperature, unreacted lignin was removed by filtration, and the final product was obtained by rotary evaporation, which was dried in vacuum at 30°C for 8 hours. The final conversion rate was 72.4%.
[0020] The resulting product is figure 1 shown.
[0021] 1782cm in raw material...
Embodiment 2
[0023] (1) Take 200g of polycondensation enzymatically hydrolyzed lignin, dry it to constant weight, put it into a pulverizer and pulverize it, and screen to obtain lignin of a certain size;
[0024] (2) Add 3 g of lignin to 100 g of water and stir, raise the temperature to 70° C., add 6 g of potassium persulfate compound salt, adjust the pH to 9, add 0.15 g of CuO to initiate the reaction, and keep warm for 7 h.
[0025] (3) Raise the temperature to 80° C., adjust the pH of the reaction solution to 11 with 50 wt % NaOH solution, add 1.5 g of 20% formaldehyde solution, and react for 4 hours.
[0026] (4) Heat up to 95°C, add 3g of sodium sulfite, and react for 7 hours. After cooling to room temperature, unreacted lignin was removed by filtration, and the final product was obtained by rotary evaporation, which was dried in vacuum at 100° C. for 12 hours. The final conversion rate was 77.3%.
Embodiment 3
[0028] (1) Take 200g of polycondensation enzymatically hydrolyzed lignin, dry it to constant weight, put it into a pulverizer and pulverize it, and screen to obtain lignin of a certain size;
[0029] (2) Add 3 g of lignin to 100 g of water and stir, raise the temperature to 60° C., add 6 g of potassium hydrogen persulfate compound salt, adjust the pH to 5, add 0.15 g of CuO to initiate the reaction, and keep warm for 5 h.
[0030] (3) Raise the temperature to 78° C., adjust the pH of the reaction solution to 9 with 20 wt % NaOH solution, add 1.5 g of 30% formaldehyde solution, and react for 2 hours.
[0031] (4) Heat up to 90°C, add 3g of sodium sulfite, and react for 5h. After cooling to room temperature, unreacted lignin was removed by filtration, and the final product was obtained by rotary evaporation, which was then vacuum-dried at 60° C. for 9 h. The final conversion rate was 71.1%.
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