Epoxy-modified trifluoropropyl silicone oil and preparation method thereof
A technology of trifluoropropyl silicon and epoxy modification, which is applied in the direction of biocide-containing paints, coatings, antifouling/underwater coatings, etc., and can solve the problem of poor reactivity of trifluoropropyl silicone oil and salt resistance Fog, chemical corrosion resistance is not good enough, trifluoropropyl silicone oil has a narrow viscosity range, etc., to achieve the effect of improving salt spray resistance, good moisture resistance, and good reactivity
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[0029] The preparation method of above-mentioned epoxy-modified trifluoropropyl silicone oil comprises the steps:
[0030] The molar ratio of dimethylcyclosiloxane, trifluoropropylcyclotrisiloxane, hydrogen-containing siloxane and vinylcyclosiloxane is 1:0.5-2:0.1-1:0- 0.1 for mixing, then add an end-capping agent for ring-opening polymerization to obtain hydrofluorosilicone oil;
[0031] The hydrogen-containing fluorosilicone oil and allyl alkyl ether are mixed according to a molar ratio of 1:1.2-1.6 to carry out a hydrosilylation reaction.
[0032] In the research process of the present invention, it is found that the existing epoxy-modified trifluoropropyl silicone oil has unsatisfactory reactivity, and the improvement of the performance of the protective coating is limited, and the reason for the narrow viscosity range is mainly due to: the traditional epoxy The preparation method of modified trifluoropropyl silicone oil leads to.
[0033] Specifically, the traditional e...
Embodiment 1
[0051] This embodiment is a preparation method of epoxy-modified trifluoropropyl silicone oil, the steps are as follows:
[0052] 1) Preparation of hydrofluorosilicone oil: Dimethylcyclosiloxane, trifluoropropylcyclotrisiloxane (D 3 F), tetramethyltetrahydrocyclotetrasiloxane (D 4 H) According to the silicon atom molar ratio 1:1:0.2 into the reactor, then add 5 parts by weight of end-capping agent (hexamethyldisiloxane) into the reactor, under the action of cation exchange resin at 70 ° C After reacting for 3 hours, the catalyst was filtered off, and the low molecular weight was removed at 120°C for 3 hours to obtain hydrofluorosilicone oil. The conversion rate was 81.0%.
[0053] 2) Preparation of epoxy-modified trifluoropropyl silicone oil: Add hydrogen-containing fluorosilicone oil and allyl glycidyl ether into the reactor at a ratio of 1:1.3, turn on the vacuum to -0.08MPa for dehydration for 1 hour, and use nitrogen to eliminate the vacuum Then heat up to 90°C, then ad...
Embodiment 2
[0056] This embodiment is a preparation method of epoxy-modified trifluoropropyl silicone oil, the steps are as follows:
[0057] 1) Preparation of hydrofluorosilicone oil: Dimethylcyclosiloxane, trifluoropropylcyclotrisiloxane (D 3 F), tetramethyltetrahydrocyclotetrasiloxane (D 4 H), trimethyltrivinylcyclotrisiloxane is added in the reactor according to the silicon atom molar ratio of 1:0.5:1:0.05, and then 1 weight part of the end-capping agent (1,1,3,3-4 Methyldisiloxane) was added into the reactor, reacted at 60°C for 4 hours under the action of cation exchange resin, filtered off the catalyst, and removed at 120°C for 3 hours to remove low molecular weight to obtain hydrofluorosilicone oil. The conversion rate was 83.2%.
[0058] 2) Preparation of epoxy-modified trifluoropropyl silicone oil: Add hydrogen-containing fluorosilicone oil and allyl glycidyl ether into the reactor at a ratio of 1:1.2, turn on the vacuum to -0.08MPa for dehydration for 1 hour, and use nitrogen...
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