Preparation method of vinyl-mono-capped fluorinated silicone raw-rubber
A vinyl-terminated, fluorosilicone rubber technology, which is applied in the field of fluorosilicone rubber raw rubber preparation, can solve the problem that vinyl-terminated monomers are difficult to participate in copolymerization, and achieve the effect of increasing vinyl content and high activity
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Embodiment 1
[0025] Will D 3 After F25g and 14g of tetramethyldivinyldisiloxane are added to the reactor for dehydration treatment, dry nitrogen is introduced, 10g of lithium hydroxide is added, and the reaction is stirred at 150°C for 4 hours to obtain a vinyl-terminated initiator.
[0026] Will D 3 After the mixture of F100g, 60g octamethylcyclotetrasiloxane and 3g tetramethyltetravinylcyclotetrasiloxane was dehydrated, 0.5g of the above-prepared initiator was added, and the polymerization was stirred at 150°C for 4 hours. Add 0.25 g of acetic acid to the obtained mixed solution, stir at 80° C. for 0.5 hours, and then raise the temperature to remove low-boiling substances to obtain a vinyl single-terminated fluorosilicone rubber raw rubber.
[0027] Perform the following performance tests on the prepared initiator and raw rubber:
[0028] 1. Test the molecular weight and distribution of fluorosilicone raw rubber
[0029] GPC was used to test the molecular weight and distribution of raw rubber. I...
Embodiment 2
[0034] Will D 3 After F15g and 14g of tetramethyldivinyldisiloxane are added to the reactor for dehydration treatment, dry nitrogen is introduced, 6g of sodium hydroxide is added, and the reaction is stirred at 120°C for 1 hour to obtain a vinyl-terminated initiator.
[0035] Will D 3 After 200g of F was dehydrated, 2.5g of the initiator prepared above was added, and the polymerization was stirred at 120°C for 2 hours. Add 1.0 g of silicon-based phosphate to the resulting mixed solution, stir at 60° C. for 2 hours, and then raise the temperature to remove low-boiling substances to obtain vinyl mono-terminated fluorosilicone rubber raw rubber.
[0036] The test items are the same as in Example 1. The test results of the molecular weight, molecular weight distribution coefficient and vinyl content of the prepared small molecule initiator and raw rubber are shown in Table 1.
Embodiment 3
[0038] Will D 3 After F25g and 12g of dimethylvinylethoxysilane are added to the reactor for dehydration treatment, dry nitrogen is introduced, 8g of tetramethylammonium hydroxide is added, and the reaction is stirred at 40°C for 0.5 hours to obtain a vinyl-terminated initiator.
[0039] Will D 3 After F200g is dehydrated, 20g of the initiator prepared above is added, and the polymerization is stirred at 40°C for 0.5 hour. 1.6 g of phosphoric acid was added to the resulting mixed solution, stirred at 40°C for 4 hours, and then heated to remove low-boiling substances to obtain a vinyl single-terminated fluorosilicone rubber raw rubber.
[0040] The test items are the same as in Example 1. The test results of the molecular weight, molecular weight distribution coefficient and vinyl content of the prepared small molecule initiator and raw rubber are shown in Table 1.
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