The preparation method of cellulose ester
A technology of cellulose ester and cellulose, which is applied in the field of chemistry and can solve problems such as long reaction time
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Embodiment 1
[0060] Embodiment 1 of the present invention: the preparation method of cellulose ester comprises the steps:
[0061] The preparation method of cellulose ester, comprises the steps:
[0062] 1) mixing cellulose, organic base and organic solvent to obtain and mix the system;
[0063] 2) Fill the mixed system with carbon dioxide and react at 30°C-100°C for 0.1-24h to obtain cellulose-based CO 2 Reversible ionic liquid compounds;
[0064] 3) To cellulose-based CO 2 adding vinyl ester to the reversible ionic liquid compound, and reacting at 20-120°C for 0.1-48 hours to obtain a reaction mixture;
[0065] 4) adding water or C1-C4 lower aliphatic alcohols to the reaction mixture, and then filtering the reaction mixture containing lower aliphatic alcohols to obtain filtered solids;
[0066] 5) Purify and dry the solid mixture obtained by filtration to obtain cellulose ester.
[0067] Its flow chart is attached figure 1 .
[0068] According to the above steps, weigh different k...
Embodiment 2
[0071] Embodiment 2 of the present invention: the preparation method of cellulose ester
[0072] According to the steps of Example 1, weigh α-cellulose 0.65g, organic base 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) 1.83g and dimethylsulfoxide (DMSO) 10g (the molar ratio of DBU to glucose units in cellulose is 3:1), put them into the autoclave together and tighten them, and feed 0.5MPa of CO 2 , stirred and reacted at 50 for 1 hour to obtain a clear and transparent cellulose solution, the concentration of the cellulose solution being 5% (mass fraction). Take 5g of the above solution and add it to a two-necked bottle, add 0.69g of vinyl benzoate under mechanical stirring at 40°C and react for 4 hours. Once, freeze-dried for 24 hours to obtain the product cellulose benzoate.
[0073] The NMR characterization and calculation of the cellulose benzoate sample showed that its degree of substitution was 2.50. See the attached NMR spectrum figure 2 . Calculated as follows:
[0074...
Embodiment 4
[0076] Embodiment 4 of the present invention: the preparation method of cellulose ester
[0077] According to the steps of Example 1, the applicability of the patent of the present invention to vinyl esters of different structures and different organic bases and the influence of reaction temperature and reaction time on the degree of substitution of cellulose esters were studied.
[0078] According to the steps of Example 1, weigh 0.65g of α-cellulose, organic base and dimethyl sulfoxide (DMSO) 10g (the molar ratio of organic base to glucose unit in cellulose is 3:1), add together Tighten to the high-pressure reactor, and introduce 0.5MPa of CO 2 , stirred and reacted at 50 for 1 hour to obtain a clear and transparent cellulose solution, the concentration of the cellulose solution being 5% (mass fraction). Take 5g of the above solution and add it to a two-necked bottle, add vinyl ester of 3 times the molar amount of cellulose under mechanical stirring, and react for a certain...
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Abstract
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