A kind of quaternized silicone oil and preparation method thereof
A technology of quaternized silicone and amino silicone oil, which is applied in fiber types, textiles and papermaking, fiber treatment, etc., and can solve problems such as the use of emulsifiers
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[0025] like figure 1 Shown, the preparation method of the quaternized silicone oil of an embodiment, comprises the steps:
[0026] S1: Add octamethylcyclotetrasiloxane, ammonia type coupling agent, end-capping agent and basic catalyst into a mixed solvent, and obtain an amino silicone oil solution by ring-opening polymerization through solution polymerization.
[0027] Specifically, add octamethylcyclotetrasiloxane, ammonia type coupling agent, basic catalyst and mixed organic solvent into a four-necked flask, and stir the above raw materials evenly at room temperature at a stirring speed of 200-400 rpm . Wherein, the four-necked flask is equipped with a stirrer, a reflux condenser and a thermometer.
[0028] After stirring evenly, heat up to a temperature of 45-75°C. At a stirring speed of 200-400 rpm and a temperature of 45-75°C, octamethylcyclotetrasiloxane and ammonia-type coupling agent are mixed in the basic catalyst Under the influence of reaction for 5-10 hours. Un...
Embodiment 1
[0061] Mix 13.0g octamethylcyclotetrasiloxane, 2.5g N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH602), 0.08g catalyst potassium hydroxide and 84g mixed solvent Put it into a four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, stir and mix evenly at a speed of 300 rmp / min, then heat up to 50°C, react for 6 hours, and finally add 0.06g of end capping agent hexamethyldisiloxane , reacted for 1.5 hours to obtain amino silicone oil solution, wherein, the mixed solvent used was a mixture of toluene and isopropanol, and its mass percentage was 20:80;
[0062] Add dimethylaminoethyl methacrylate to the obtained aminosilicone oil solution, stir and mix evenly at a speed of 300 rmp / min, then heat up to 25 ° C and react for 15 hours to obtain a modified aminosilicone oil solution, wherein the primary aminosilicone oil The molar ratio of amine to dimethylaminoethyl methacrylate was 1:1.
[0063] Under stirring at room temperature and at a speed of 3...
Embodiment 2
[0067] 10.0g octamethylcyclotetrasiloxane, 4g N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane (KH602), 0.08g catalyst potassium hydroxide and 84g mixed solvent were added In a four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, stir and mix evenly at a speed of 300 rmp / min, then heat up to 50 ° C, react for 6 hours, and finally add 0.06 g of end capping agent hexamethyldisiloxane, The reaction was carried out for 1.5 hours to obtain an amino silicone oil solution, wherein the mixed solvent used was a mixture of toluene and isopropanol, and its mass percentage was 20:80;
[0068] Add dimethylaminoethyl methacrylate to the obtained aminosilicone oil solution, stir and mix evenly at a speed of 300 rmp / min, then heat up to 25 ° C and react for 15 hours to obtain a modified aminosilicone oil solution, wherein the primary aminosilicone oil The molar ratio of amine to dimethylaminoethyl methacrylate was 1:1.
[0069] Under stirring at room temperatur...
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