Method for preparing modified polymerization initiator by using continuous reactor
A technology of polymerization initiator and reactor is applied in the field of preparing modified polymerization initiator, which can solve the problem of high manufacturing cost, and achieve the effects of reducing defects, reducing the generation of by-products, and improving the conversion rate.
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[0052] The method for preparing a modified polymerization initiator according to an embodiment of the present invention is characterized in that it includes the step of reacting a compound represented by the following formula 1 with a compound represented by the following formula 2 (step A), wherein the reaction includes the first continuous Channel and the continuous reactor of the second continuous channel, and before carrying out the reaction, the compound represented by formula 1 is injected into the continuous reactor through the first continuous channel and the compound represented by formula 2 is injected into the continuous reaction through the second continuous channel In the device:
[0053] [Formula 1]
[0054]
[0055] In formula 1,
[0056] X is -NR a R b , -OR c or -SR d ,and
[0057] R a to R d Each independently is an alkyl group having 1 to 30 carbon atoms, an alkenyl group having 2 to 30 carbon atoms, an alkynyl group having 2 to 30 carbon atoms, a...
Embodiment 1
[0150] Prepare two 2 L vacuum-dried stainless steel pressure vessels. Into the first pressure vessel, 1822 g of hexane, 250 g of a compound represented by the following formula 1-1, and 162 g of tetramethylethylenediamine were injected to prepare a first reaction solution. At the same time, 385 g of liquid 2.5 M n-butyllithium (in hexane) and 1845 g of hexane were injected into the second pressure vessel to prepare a second reaction solution. In this case, the molar ratio of the compound represented by Formula 1-1, n-butyllithium, and tetramethylethylenediamine was 1:1:1. The pressure of each pressure vessel is maintained at 5 bar, and the first reaction solution is injected into the continuous reactor through the first continuous channel at an injection rate of 1.0 g / min, and the injection rate of 1.0 g through the second continuous channel is injected into the continuous reactor using a mass flow meter. / min injection rate into the second reaction solution. In this case, t...
Embodiment 2
[0155] Prepare two 2 L vacuum-dried stainless steel pressure vessels. Into the first pressure vessel, 1900 g of hexane, 250 g of a compound represented by the following formula 1-5, and 124 g of tetramethylethylenediamine were injected to prepare a first reaction solution. At the same time, 385 g of liquid 2.5 M n-butyllithium (in hexane) and 2600 g of hexane were injected into the second pressure vessel to prepare a second reaction solution. In this case, the molar ratio of the compound represented by Formula 1-5, n-butyllithium, and tetramethylethylenediamine was 1:1:1. The pressure of each pressure vessel is maintained at 5 bar, and the first reaction solution is injected into the continuous reactor through the first continuous channel at an injection rate of 1.0 g / min, and the injection rate of 1.0 g through the second continuous channel is injected into the continuous reactor using a mass flow meter. / min injection rate into the second reaction solution. In this case, t...
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