Epoxy resin and preparation method thereof
A technology of epoxy resin and polymer, applied in the direction of adhesive type, polyether adhesive, coating, etc., can solve the problems of epoxy resin process difficulties, poor solubility, large usage, etc., and avoid solvent recovery Difficulty, low cost, effect of improving solubility
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[0043] The present invention also provides a preparation method of epoxy resin, comprising: a) mixing hydroquinone represented by formula V, formula VI or formula VII with 4,4'-difluorobenzophenone, alkali metal carbon The acid salt is mixed in an organic solvent, and a polymerization reaction is carried out to obtain a polymer; b) the polymer obtained in step a) is mixed with acetic anhydride and hydrogen peroxide, heated, stirred and oxidatively added to obtain the epoxy resin shown in formula I; wherein R is a repeating unit represented by formula II, formula III or formula IV, R 1 , R 2 respectively methyl or hydrogen, n=1~20;
[0044]
[0045] Formula V Formula VI Formula VII.
[0046] The hydroquinone described in formula V, VI, VIII of the present invention is prepared by the following method, and the preparation method of the hydroquinone shown in formula V is:
[0047]
[0048] Combining cyclopentadiene with R 1 and / or R 2 The p-benzoquinone is mixed with D...
Embodiment 1
[0060]
[0061] Formula 1
[0062] The epoxy resin represented by formula 1 wherein n is 20 was prepared.
[0063] Equipped with stirring device, thermometer, water separator, condenser tube and N 2 Add hydroquinone shown in formula V in the reaction bottle of gas protection device, wherein R 1 , R 2 All hydrogen 17.4g, 0.1mol, 4,4-difluorobenzophenone 21.8g, 0.1mol, potassium carbonate 27.6g, 0.2mol, 150mL DMF and toluene 70mL. Stir, heat, and reflux the water with toluene at 120°C for 3.5h, release the toluene and the generated water in the water separator, slowly raise the temperature to 160°C, polymerize for 1.5h, pour the product into water, suction filter, and use Washed three times with deionized water and dried in a vacuum oven for 24 hours to obtain a polymer.
[0064] Take 10g of the obtained polymer and dissolve it in 50mL DMF, add 50mL acetic anhydride and 70% hydrogen peroxide, stir at 80°C for 6h, pour into ice water after cooling, filter with suction, was...
Embodiment 2
[0069]
[0070] Formula 2
[0071] An epoxy resin represented by formula 2, where n=2, was prepared.
[0072] Equipped with stirring device, thermometer, water separator, condenser tube and N 2 Add hydroquinone 25.2g, 0.1mol, R 1 is methyl, R 2 Both are hydrogen, 21.8g, 0.1mol of 4,4-difluorobenzophenone, potassium carbonate (27.6g, 0.2mol), 150mL of DMF and 70mL of toluene. Stir, heat, and reflux with toluene at 120°C to carry water for 3.5 hours, release toluene and generated water in the water separator, slowly raise the temperature to 160°C, polymerize for 2 hours, pour the product into water, filter with deionization Washed with water three times, dried in a vacuum oven for 24 hours to obtain a polymer.
[0073] Dissolve 10 g of the obtained polymer in 50 mL of DMF, add 50 mL of acetic anhydride and 70% hydrogen peroxide, stir at 80°C for 6 h, pour into ice water after cooling, filter with suction, wash with deionized water and dry in vacuum for 12 h to obtain a co...
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