A kind of ternary iron catalyst and its application to prepare polymer by catalyzing the copolymerization of epichlorohydrin and butadiene
A technology of epichlorohydrin and catalyst, which is applied in the field of polymer synthesis to achieve the effect of high yield
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Embodiment 1
[0019] In a two-necked flask equipped with a thermometer and a stirring rotor, add 20 ml of hexane treated with anhydrous and anaerobic treatment, and start stirring, and then sequentially introduce 1.5 ml of butadiene and 6.0 ml of epichlorohydrin. After heating in a water bath at 70°C for 15 minutes, add 0.5mL iron isooctanoate solution (0.1mol / L hexane solution), 0.25mL triethylaluminum solution (1mol / L hexane solution), 0.5mL Diethyl phosphite solution (0.2mol / L hexane solution). Put the polymerization bottle into a 70°C water bath and react for 2 hours. After the reaction finishes, add 5% hydrochloric acid ethanol solution to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methylphenol Mixed at a weight ratio of 1:1), weighed after drying, the polymer yield was 45.0%. The polymer sample was tested by GPC, and the number average molecular weight o...
Embodiment 2
[0021] In a two-necked flask equipped with a thermometer and a stirring rotor, 20 ml of hexane treated with anhydrous and anaerobic treatment was metered in, and the stirring was started, and then 6 ml of butadiene and 1.5 ml of epichlorohydrin were sequentially introduced. After heating in a water bath at 60°C for 15 minutes, add 0.6 mL of iron acetylacetonate solution (0.1 mol / L hexane solution), 1.2 mL of sesquialuminum solution (1 mol / L hexane solution), and 0.6 mL of three o-methylphenyl phosphite solution (0.2mol / L hexane solution), put the polymerization bottle into a water bath at 60°C, and react for 4 hours. After the reaction, add 5% ethanol solution of hydrochloric acid to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), weighed after drying, and the polymer yield was 65.0%. The polymer sampl...
Embodiment 3
[0023] In a two-necked flask equipped with a thermometer and a stirring rotor, 20 ml of hexane treated with anhydrous and anaerobic treatment was metered in, and the stirring was started, and then 6 ml of butadiene and 1.5 ml of epichlorohydrin were sequentially introduced. After heating in a water bath at 70°C for 15 minutes, add 0.5ml iron isooctanoate solution (0.1mol / L hexane solution), 1.0mL triisobutylaluminum solution (1mol / L hexane solution), 0.5ml mL of diethyl phosphite solution (0.2mol / L hexane solution), put the polymerization bottle into a water bath at 70°C, and react for 2 hours. After the reaction, add 5% ethanol solution of hydrochloric acid to terminate the polymerization, pour out the supernatant, and the obtained polymer is washed with a large amount of ethanol, and anti-aging agent (1010 and 2,6-di-tert-butyl-4-methyl Phenol was mixed at a weight ratio of 1:1), weighed after drying, and the polymer yield was 70.0%. The polymer sample was tested by GPC, an...
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