A kind of low hydrogen-containing silicone oil, organosilicon surfactant and its preparation method and application
A technology of low-hydrogen-containing silicone oil and high-hydrogen-containing silicone oil, which is applied in the fields of low-hydrogen-containing silicone oil, silicone surfactant and its preparation, and polyurethane, and can solve the problem of increased cost, decreased surface tension, activity, and foam stability of surfactants and other problems to achieve the effect of improving odor, realizing porosity and stability, and reducing volatilization
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Embodiment 1
[0048] The preparation method of embodiment 1 hydrogen-containing silicone oil intermediate
[0049] Add 6g of MD 5 M(M means (CH 3 ) 3 SiO 1 / 2 , D means (CH 3 ) 2 SiO), 230g octamethylcyclotetrasiloxane (abbreviated as D 4 ), 16g high hydrogen silicone oil MD 50 M; After starting to stir for half an hour, add 3g of concentrated sulfuric acid catalyst with a mass percentage concentration of 93%, start stirring, nitrogen protection, use a heating mantle to heat to 25°C, stir for 36 hours, then add 12g of sodium bicarbonate, 3g of activated carbon, continue Stir for 2 hours, obtain hydrogen-containing silicone oil MD after vacuum filtration 95 D' 8 M, with a hydrogen content of 23cc H 2 / g, the molecular weight of Example 1 measured by gel permeation chromatography (GPC) is 7538, which is basically consistent with the design molecular weight of 7688, and the GPC data are shown in the following table.
[0050]
Embodiment 2
[0051] The preparation method of embodiment 2 low hydrogen-containing silicone oil
[0052] Add 45.6g MD 5 M(M means (CH 3 ) 3 SiO 1 / 2 , D means (CH 3 ) 2 SiO), the hydrogen-containing silicone oil intermediate (MD) of 270g embodiment 1 95 D' 8 M), 17.3g high hydrogen silicone oil MD 53 M; After starting to stir for half an hour, add 4g of acidic ion exchange resin, start stirring, nitrogen protection, use a heating mantle to heat to 25°C, stir for 36 hours, then add 16g of sodium bicarbonate, 5g of activated carbon, continue to stir for 2 hours, and vacuum filter After obtaining low hydrogen silicone oil MD 25 D' 4 M (see Figure 7 NMR silicon spectrum), the hydrogen content is 40ccH 2 / g, the relative molecular weight of Example 2 measured by gel permeation chromatography (GPC) is 2291g / mol, which is basically consistent with the design molecular weight of 2256g / mol, and the GPC data are shown in the table below.
[0053]
Embodiment 3
[0054] The preparation method of embodiment 3 low volatile silicone surfactants
[0055] In a 250ml four-necked flask with a fixture, constant temperature function, mechanical stirring, thermocouple and nitrogen, add 76g of low hydrogen-containing silicone oil (Example 2); 75g of allyl alcohol starting, methyl-capped Polyoxyethylene ether with an average molecular weight at the end of about 7460, which contains 50% by mole of ethylene oxide groups and 50% by mole of propylene oxide groups (herein, referred to as polyether A); add 100g of allyl Alcohol-initiated, methyl-terminated polyoxyethylene ether with an average molecular weight of about 1700, which contains 50 mole percent of ethylene oxide groups and 50 mole percent of propylene oxide groups (herein, referred to as polyoxyethylene groups) Ether B), start to stir, adopt heating mantle to be heated to 80 ℃, stir for 5 minutes, add the chloroplatinic acid ethanol solution of 30ppm Pt, after reacting for 4 hours, this produ...
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