Organopolysilmethylene and a composition comprising the same
A technology of polymethylene siloxane and polysiloxane, which is applied in the field of organopolymethylene siloxane and organopolymethylene siloxane composition, can solve the problem of poor processability, expensive, Difficult to synthesize and other problems, to achieve the effect of excellent heat resistance
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[0086] Hereinafter, examples and comparative examples are shown to explain the present invention in more detail, but the present invention is not limited to the following examples. In addition, in the following content, "parts" means parts by weight, Me means methyl, and Vi means vinyl.
example 1
[0088] (A1) Synthesis of alkenyl-containing organopolymethylene siloxane
[0089] Dissolve 1540 g (4.64 mol, 90 mol%) of chlorine-containing methylene silicon of the following formula (6) and 54.2 g (0.45 mol, 10 mol%) of dimethylvinyl monochlorosilane of the following formula (7) In 1000 g of xylene, it was added dropwise to a mixed solvent system of 600 g of water and 300 g of xylene at 60°C to perform a hydrolysis reaction. Then, after the maturation reaction was performed at room temperature for 3 hours, the waste acid was separated, washed with water, and azeotropic dehydration was performed at 140°C.
[0090] [化11]
[0091]
[0092] [化12]
[0093]
[0094] 0.2g of KOH was added to the polymethylene silicate with the introduction of alkenyl groups, and the reaction was carried out at 140°C for 10 hours to carry out alkali polymerization, followed by neutralization, filtration, and separation at 160°C / 5mmHg for 30 minutes. ). As a result of analysis by 1H-NMR, it was found that...
example 2
[0098] (A2) Synthesis of alkenyl-containing organopolymethylene siloxane
[0099] Combine 260.3 g (0.335 mol, 67 mol%) of chlorine-containing methylene silicon of the following formula (9) and 19.9 g (0.165 mol, 33 mol%) of dimethylvinyl monochlorosilane of the above formula (7) with Example 1 was similarly dissolved in 200 g of xylene, and was added dropwise to a mixed solvent system of 200 g of water and 100 g of xylene at 60° C. to perform a hydrolysis reaction. Then, the maturation reaction was carried out at room temperature for 5 hours. Then the waste acid is separated, washed with water, and azeotropic dehydration is performed at 140°C. 0.2g of KOH was added to the polymethylene silicate with the introduction of alkenyl groups, reacted at 140°C for 10 hours to carry out alkali polymerization, and then neutralized and filtered, and then separated at 160°C / 5mmHg for 30 minutes. The alkenyl group-containing organopolymethylene silicone siloxane (A2) of the following formu...
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