Preparation method for phenyl hydrogen-containing silicone oil
A technology of phenyl hydrogen-containing silicone oil and phenyl alkoxysilane, applied in chemical instruments and methods, petroleum industry, pharmaceutical formulations, etc. Problems such as poor repeatability, to achieve the effect of easy control, simple operation and mild conditions
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[0024] Example 1
[0025] The preparation method of phenyl hydrogen-containing silicone oil in this embodiment sequentially includes the following steps:
[0026] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, and add organic solvent, water and end-capping agent, and carry out hydrolysis and polycondensation reaction under the action of acid catalyst;
[0027] The above-mentioned phenyl alkoxy silane is phenyl trimethoxy silane, and the amount thereof is 14.50 g (0.0731 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its dosage is 10.67g (0.0443mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total moles of phenyl groups to the total moles of Si-H groups is about 0.413:1.
[0028] The above-mentioned organic solvent is toluene, and its amount is 40.00 g. The amount of organic solvent is about 1.59 times the total mass of the basic reaction monomer.
[0029] The above-mentioned water is deionized water, a...
Example Embodiment
[0038] Example 2
[0039] The preparation method of phenyl hydrogen-containing silicone oil in this embodiment sequentially includes the following steps:
[0040] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, and add organic solvent, water and end-capping agent, and carry out hydrolysis and polycondensation reaction under the action of acid catalyst;
[0041] In this step (1), the hydrolysis polycondensation reaction is carried out under stirring, the reaction time of the hydrolysis polycondensation reaction is 10 hours, and the reaction temperature is 100°C.
[0042] The above-mentioned phenyl alkoxy silane is phenyl trimethoxy silane, and the amount thereof is 19.80 g (0.0999 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its dosage is 2.60g (0.0108mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total moles of phenyl groups to the total moles of Si-H groups is 2.3125:1.
[0043] The above-mentioned o...
Example Embodiment
[0051] Example 3
[0052] The preparation method of phenyl hydrogen-containing silicone oil in this embodiment sequentially includes the following steps:
[0053] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, and add organic solvent, water and end-capping agent, and carry out hydrolysis and polycondensation reaction under the action of acid catalyst;
[0054] In this step (1), the hydrolysis polycondensation reaction is carried out under stirring, the reaction time of the hydrolysis polycondensation reaction is 14 hours, and the reaction temperature is 20°C.
[0055] The above-mentioned phenyl alkoxy silane is phenyl trimethoxy silane, and the amount thereof is 19.80 g (0.0999 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its dosage is 4.16g (0.0173mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total number of moles of phenyl groups to the total number of moles of Si-H groups is about 1.44:1.
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