Method for preparing carbonic ester-carbamate mixed ester based on cellulose carbonic ester
A technology of carbamate and carbonate, applied in the field of preparation of mixed ester materials, can solve the problems of cellulose carbonate derivative literature and patent reports, type restrictions, etc.
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Embodiment 1
[0107] Weigh 1.00 g of cellulose carbonates with different substitution structures in a flask, take 5 mL of dimethyl sulfoxide (DMSO), and heat to dissolve at 50° C. Add 1.165 mL of p-toluene isocyanate and 10 wt % DBU relative to cellulose carbonate as a catalyst, and react at 50° C. for 3 h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:
[0108] Table 1 Reaction of cellulose carbonates with different structures
[0109]
[0110] where DS C1 and DS C2 Respectively represent the degree of substitution of carbonate groups of pure cellulose carbonate and the reacted cellulose carbonate-urethane mixed ester. discover DS C2 The value is generally higher than the DS C1 Large, due to NMR calculation errors.
[0111] This example fully demonstrates that for cellulose carbonates of different structures, cellulose carbonate-urethane mixed este...
Embodiment 2
[0113] Weigh 1.00 g of cellulose hexyl carbonate into a flask, take different volumes of dimethyl sulfoxide (DMSO), and heat to dissolve at different temperatures. Add 1.165mL of p-toluene isocyanate, and catalysts of different types and different mass fractions, and react at 50°C for 3h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:
[0114] Table 2 Study of different cellulose carbonate concentrations, temperatures and organic solvents
[0115]
[0116] a: ratio content of cellulose carbonate to solvent (W / V); b: dissolution temperature of cellulose carbonate; c: dissolution reagent used.
[0117] This example fully demonstrates that for different cellulose carbonate concentrations, as well as dissolution temperature and dissolution reagents, the reaction with isocyanate reagents can be realized, and finally a carbonate-urethane mixed ce...
Embodiment 3
[0119] Based on the fact that ionic liquid is a good solvent with good stability and wide adaptability, it is also a good catalyst for organic reactions. Ionic liquid has both the functions of solvent and catalyst, and a series of researches are carried out on this.
[0120] Weigh 1.00 g of cellulose hexyl carbonate into a flask, take different ionic liquids (Ionic Liquid), and heat to dissolve at different temperatures. Add 1.165mL of p-toluene isocyanate and react at 50°C for 3h. After the end, use 100 mL of water for precipitation, wash with suction and filter 3 times, and freeze-dry to obtain the product. The relevant results are shown in the table below:
[0121] Table 3 Ionic Liquids as Solvents
[0122]
[0123] a: ratio of cellulose carbonate to ionic liquid (W / W); b: dissolution temperature of cellulose carbonate; c: ionic liquids with different structures.
[0124] In conjunction with Example 2, examples fully demonstrate that ionic liquids have good solubility...
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