A kind of preparation method of carboxylated nano-cellulose whisker modified waterborne polyurethane
A technology of nanocellulose and water-based polyurethane, which is applied in the field of water-based polyurethane preparation, can solve problems such as pollution, and achieve the effects of obvious mechanical properties, improved thermal stability, and improved mechanical properties
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Embodiment 1
[0027] A kind of preparation method of carboxylated nano cellulose whisker modified waterborne polyurethane, comprises the following steps:
[0028] (1) Synthesis of carboxylated nanocellulose whiskers: dry microcrystalline cellulose in vacuum at 50°C, then mix microcrystalline cellulose, TEMPO, sodium bromide, and sodium hypochlorite solution (mass fraction 10%) at a ratio of 1:0.025 : 0.25: 100 (g / g / g / mL) ratio mixed together, stirred at 500 rpm at 20°C for reaction, adding sodium hydroxide solution during the reaction to control the pH at 10.5, until the value of pH Change again to terminate the reaction (monitor the reaction by a pH meter), centrifuge and wash the prepared mixed solution 3 times at 12000 rpm, and then dry in an oven at 60°C for 24 hours to obtain carboxylated nanocellulose whiskers .
[0029] (2) After drying 38.92g isophorone diisocyanate and 47.88g castor oil in a vacuum drying oven at 100°C for 24 hours, they were added to the reaction kettle successiv...
Embodiment 2
[0035] A kind of preparation method of carboxylated nano cellulose whisker modified waterborne polyurethane, comprises the following steps:
[0036] (1) Synthesis of carboxylated nanocellulose whiskers: Microcrystalline cellulose was vacuum-dried at 50°C, and then microcrystalline cellulose, TEMPO, sodium bromide, and sodium hypochlorite solution (mass fraction 15%) were mixed at a ratio of 1:0.025 :: 0.25: 100 (g / g / g / mL) ratio mixed together, stirred reaction at 550 rpm at 20°C, adding sodium hydroxide solution during the reaction to control the pH at 11.0, to the value of pH If there is no change, the reaction is terminated (the reaction is monitored by a pH meter), and the prepared mixed solution is centrifuged and washed 3 times at 12,000 rpm, and then dried in an oven at 60° C. for 30 hours to obtain carboxylated nanocellulose.
[0037] (2) After drying 41.7g isophorone diisocyanate and 51.3g castor oil in a vacuum oven at 100°C for 24 hours, they were added to the reacto...
Embodiment 3
[0043] A kind of preparation method of carboxylated nano cellulose whisker modified waterborne polyurethane, comprises the following steps:
[0044] (1) Synthesis of carboxylated nanocellulose whiskers: dry microcrystalline cellulose in vacuum at 60°C, then mix microcrystalline cellulose, TEMPO, sodium bromide, and sodium hypochlorite solution (mass fraction 20%) at a ratio of 1:0.025 :: 0.25: 150 (g / g / g / mL) ratio mixed together, stirred reaction at 25°C at 600 rpm, adding sodium hydroxide solution during the reaction to control the pH at 11.0, to the value of pH If there is no change, the reaction is terminated (the reaction is monitored by a pH meter), and the prepared mixed solution is centrifuged and washed 3 times at 13,000 rpm, and then dried in an oven at 60° C. for 36 hours to obtain carboxylated nanocellulose.
[0045] (2) After drying 41.51g isophorone diisocyanate and 51.07g castor oil in a vacuum oven at 100°C for 24 hours, they were added to the reactor successive...
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