A kind of preparation method of bis(alkyl polyoxyalkylene ether) secondary amine
A technology of alkyl polyoxyalkylene ether and primary amino polyoxyalkylene monoalkyl ether, which is applied in the field of preparation of bis-secondary amines, can solve the problems of inability to prepare secondary amine content and lack of secondary amines, achieve less side reactions, The effect of convenient feeding and cost reduction
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example 1
[0046] Add 200g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 10g of catalyst Raney nickel into a 500ml four-necked flask equipped with a stirrer, a thermometer, a gas conduit, and a straight condenser tube. The molecular weight of ethylenic mono-n-butyl ether is 1646, n(EO):n(PO)=3:1, and the amination rate is 70%. Hydrogen gas was passed through at a flow rate of 110 ml / min, and the temperature was raised to 180° C. at a stirring speed of 300 r / min, and reacted for 5 h.
[0047] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration, and the secondary amine content (S%) was 52%.
example 2
[0049] Add 200g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 10g of catalyst Raney nickel into a 500ml four-necked flask equipped with a stirrer, a thermometer, a gas conduit, and a straight condenser tube. The molecular weight of alkenyl n-butyl ether is 1646, n(EO):n(PO)=3:1, and the amination rate is 70%. Hydrogen gas was passed through at a flow rate of 100 ml / min, and the temperature was raised to 180° C. at a stirring speed of 300 r / min, and reacted for 5 h.
[0050] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration. The secondary amine content (S%) was 59%.
example 3
[0052] Add 1000g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 30g of catalyst Raney nickel into a 2000ml four-necked flask equipped with a stirrer, thermometer, gas conduit, and straight condenser tube. The molecular weight of ethylenic mono-n-butyl ether is 1420, n(EO):n(PO)=3:1, and the amination rate is 92%. Pass hydrogen gas at a flow rate of 200ml / min, raise the temperature to 200°C at a stirring speed of 300r / min, and react for 10h.
[0053] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration, and the secondary amine content (S%) was 54%.
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