Preparation technique of medium/high-viscosity dimethyl silicone oil
A technology of dimethyl silicone oil and preparation process, which is applied in the field of preparation technology of medium and high viscosity dimethyl silicone oil, can solve problems such as increasing product cost, and achieve the effects of reducing pollution, improving strength and good selectivity
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[0021] Example 1
[0022] (1) Catalyst preparation:
[0023] Add 100Kg of chloromethylated polystyrene spheres, 300Kg of trimethylamine aqueous solution, and 30Kg of perfluoro tertiary amine to the 1000L reaction kettle; react at 50°C for 15h, the reaction is over, filter, dry, add 20Kg of potassium hydroxide, add anhydrous Methanol 300Kg was reacted at 40°C for 13h to obtain potassium hydroxide-loaded perfluoroquaternary ammonium strong basic anion exchange resin.
[0024] (2) the synthetic reaction of dimethicone:
[0025] Add octamethylcyclotetrasiloxane (D4) 100Kg, hexamethyldisiloxane (MM) 2Kg in 1000L reactor 15Kg of cationic anion exchange resin, react for 10h at a temperature of 60°C, and then extract low boilers under reduced pressure. Cool down to obtain dimethicone, and the reaction yield and the viscosity of dimethicone are shown in Table 1.
Example Embodiment
[0026] Example 2
[0027] (1) Catalyst preparation:
[0028] Add 100Kg of chloromethylated polystyrene spheres, 200Kg of trimethylamine aqueous solution, and 10Kg of perfluoro tertiary amine into a 1000L reaction kettle; react at 40°C for 20h, the reaction is over, filter, dry, add 10Kg of potassium hydroxide, add anhydrous Methanol 100Kg was reacted at 20°C for 20h to obtain potassium hydroxide-loaded perfluoroquaternary ammonium strongly basic anion exchange resin.
[0029] (2) the synthetic reaction of dimethicone:
[0030] Add 100Kg of octamethylcyclotetrasiloxane (D4) and 0.2Kg of hexamethyldisiloxane (MM) into the 1000L reaction kettle, and the potassium hydroxide-loaded perfluoroquaternary ammonium type strong Basic anion exchange resin 15Kg, at a temperature of 40 ℃, react for 15h, and then extract low boilers through reduced pressure. Cool down to obtain dimethicone, and the reaction yield and the viscosity of dimethicone are shown in Table 1.
Example Embodiment
[0031] Example 3
[0032] (1) Catalyst preparation:
[0033] Add 100Kg of chloromethylated polystyrene spheres, 500Kg of trimethylamine aqueous solution, and 50Kg of perfluoro tertiary amine into a 1000L reaction kettle; react at 70°C for 10h, the reaction is over, filter, dry, add 10Kg of potassium hydroxide, add anhydrous Methanol 500Kg was reacted at 50°C for 10h to obtain potassium hydroxide-loaded perfluoroquaternary ammonium strongly basic anion exchange resin.
[0034] (2) the synthetic reaction of dimethicone:
[0035] In the 1000L reactor, add 100Kg of octamethylcyclotetrasiloxane (D4), 10Kg of hexamethyldisiloxane (MM), and the perfluorinated quaternary ammonium type strong base of the loaded potassium hydroxide prepared in step (2). 15Kg of cationic anion exchange resin, react for 5h at a temperature of 80℃, and then extract low boilers under reduced pressure. Cool down to obtain dimethicone, and the reaction yield and the viscosity of dimethicone are shown in Ta...
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