Fluorine-containing organosilicon polymer and preparation method thereof
A polymer and organosilicon technology, which is applied in the field of organic silicon fluorine polymer materials and fine chemicals, can solve the problems of long carbon chain fluoroalkyl groups that are not environmentally friendly and cumulatively toxic, not refractory, and not cumulatively toxic. Achieve the effects of environmentally friendly surface activity, high fluorine content, and low surface tension
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Embodiment 1
[0049] In a four-necked flask equipped with a reflux condenser, mechanical stirring and heating device, put 400 grams of 3-tridecafluorohexylpropene and 500 grams of tridecafluoro-1-iodohexane, and heat the mixture to 88 ° C, under nitrogen protection 10 g of initiator azobisisobutyronitrile was added, and the reaction mixture was stirred and reacted at 88° C. for 48 hours. During this period, azobisisobutyronitrile was added 3 times, and 2 g of azobisisobutyronitrile was added each time. After the reaction is over, stop the reaction, and rectify (the temperature is 150°C, the vacuum degree is 2mmHg) to obtain a fraction at 106-107°C, which is the product 1,3-bis(tridecafluorohexyl)-2-iodopropane, with a yield of 97.0 %.
[0050] In a three-necked flask equipped with a reflux condenser, a thermometer, and a constant pressure dropping funnel, add 2.9 grams of magnesium chips and 50 grams of anhydrous tetrahydrofuran, introduce nitrogen, start stirring with a magnetic stirrer, a...
Embodiment 2
[0067] Bis[1,3-bis(tridecafluorohexyl)isopropyl]dichlorosilane was prepared according to Example 1.
[0068] Preparation of Polyfluoroalkyl Polysiloxanes by Cohydrolysis-Equilibrium Polycondensation
[0069]In a three-necked flask equipped with a reflux condenser, a thermometer and a constant pressure dropping funnel, 60 grams of water and 180 grams of dichloromethane were added successively. ) isopropyl] dichlorosilane, 12.6 grams of dimethyldichlorosilane and 2.5 grams of trimethylchlorosilane are mixed uniformly and added dropwise through a constant pressure dropping funnel, and the drops are completed in 2 hours. After the dropwise addition, the reaction solution is heated up The reaction was continued for 5 hours at room temperature. The reaction solution was poured into a separatory funnel, and the acid water in the lower layer was removed. The oil layer was washed 3 times with a 5% sodium hydroxide aqueous solution with a mass concentration of 40 grams of sodium hydrox...
Embodiment 3
[0078] Bis[1,3-bis(tridecafluorohexyl)isopropyl]dichlorosilane was prepared according to Example 1.
[0079] In a three-necked flask equipped with a reflux condenser, a thermometer and a constant pressure dropping funnel, 60 grams of water and 200 grams of dichloromethane were added successively. ) isopropyl] dichlorosilane, 25.2 grams of dimethyldichlorosilane and 2.7 grams of trimethylchlorosilane are uniformly mixed and then added dropwise through a constant pressure dropping funnel, and the drops are completed in 2 hours. After the dropwise addition, the reaction solution is heated The reaction was continued for 5 hours at room temperature. The reaction solution was poured into a separatory funnel, and the acid water in the lower layer was removed. The oil layer was washed 3 times with a 5% sodium hydroxide aqueous solution with a mass concentration of 40 grams of sodium hydroxide aqueous solution, and then washed 5 times with deionized water. Use 50 grams of deionized wa...
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