A kind of preparation method of water-resistant cellulose-based adhesive
A cellulose-based, cellulose-based technology, applied in the direction of adhesives, adhesive types, grafted polymer adhesives, etc., can solve the problems of toxicity and poor water resistance, and achieve good adhesion and water resistance
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[0014] A water-resistant cellulose-based adhesive, the preparation method of which comprises the following steps:
[0015] a, the synthesis of cellulose-based macromolecular initiator: Lithium chloride / N,N - After the dimethylacetamide is dissolved, add pyridine and 2-bromoisobutyryl bromide dropwise, react at room temperature for 24 hours, filter, and dry in vacuum to obtain a bromine-containing cellulose-based macromolecular initiator;
[0016] b, preparation of water-resistant cellulose-based adhesive: the brominated cellulose-based macromolecular initiator, dopa monomer and acrylic monomer prepared in step a are added to N,N -Dimethylformamide, cuprous bromide, N , N , N ', N ', N In a mixed solution of ''-pentamethyldiethylenetriamine, in N 2 Copolymerize under the condition of 60°C to obtain a protected adhesive, and finally deprotect it with hydrochloric acid to obtain a water-resistant cellulose-based adhesive.
Embodiment 1
[0023] Add 2g (12.4mmol) cellulose to 200mL of 5-10g / 100mL N , N - Dimethylacetamide / lithium chloride solution, heated to 100° C. and stirred for 2 hours in an oily pan, then stirred at room temperature for one day to obtain a cellulose solution. Under ice-bath conditions, 5.0 mL (62.1 mmol) of pyridine and 7.7 mL (62.1 mmol) of 2-bromoisobutyryl bromide were added and reacted at room temperature for 24 h. After the reaction was completed, precipitated with 4L of absolute ethanol, and dried in a vacuum to obtain a cellulose-based macromolecular initiator, whose degree of substitution was calculated to be 0.85.
[0024] Weigh 0.311g (1 mmol) cellulose-based macromolecular initiator, dissolve in 25mL N , N - In dimethylformamide, after it dissolves, add 0.636mL (6 mmol) methyl methacrylate and 1.35g (3 mmol) dopa monomer, then add 0.144g cuprous bromide and 0.63mL N , N , N ', N ', N ''-pentamethyldiethylenetriamine, charged with N 2 , reacted at 60°C for 12 hours, and ...
Embodiment 2
[0026] Add 3g (18.6mmol) cellulose to 250mL of 5-10g / 100mL N , N - Dimethylacetamide / lithium chloride solution, heated to 100° C. and stirred for 2 hours in an oily pan, then stirred at room temperature for one day to obtain a cellulose solution. Under ice bath conditions, 7.5mL (93.1mmol) of pyridine and 11.5mL (93.0mmol) of 2-bromoisobutyryl bromide were added and reacted at room temperature for 24h. After the reaction was completed, precipitated with 5L of absolute ethanol, and dried in vacuum to obtain a cellulose-based macromolecular initiator, and its degree of substitution was calculated to be 0.83.
[0027] Weigh 0.311g (1 mmol) cellulose-based macromolecular initiator, dissolve in 25mL N , N - In dimethylformamide, after it dissolves, add 0.742mL (7 mmol) methyl methacrylate and 0.90g (2 mmol) dopa monomer, then add 0.144g cuprous bromide and 0.63mL N , N , N ', N ', N ''-pentamethyldiethylenetriamine, charged with N 2 , reacted at 60° C. for 12 hours, and fi...
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