Method for radical polymerization of ethylenically unsaturated compounds
An unsaturated compound technology, applied in the field of free radical polymerization of ethylenically unsaturated compounds, can solve problems such as slow cost, and achieve the effects of low cost in industrial scale, shortened polymerization time, and easy control.
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Embodiment 1
[0255] In a 10-liter stainless steel laboratory reactor equipped with a 3-stage InterMIG stirrer (operating at 150 rpm), a thermometer and a reflux condenser, 1604.1 g of mineral oil of the third group class (e.g. from Fortum Corporation) were initially charged. Nexbase 3020) and 4125.0 g of a monomer mixture consisting of: methacrylic acid C in a weight ratio of 86.5:3.5:10.0 12 -C 18 Alkyl esters, dimethylaminopropyl methacrylamide and methyl methacrylate (MMA), together with 5.6 g of dodecylmercaptan. The temperature was adjusted to 110°C. Afterwards, 10.3 g of tert-butyl peroctoate were metered in over 2 hours, with 22% of the given amount being added in the first hour and 78% of the given amount being added in the second hour. Thirty minutes later, an additional 4.1 g of tert-butyl peroctoate was added. For better handling and for stabilization, 1770.9 g of 100N oil and 15.0 g of 4-methyl-2,6-di-tert-butylphenol were also added. The total reaction time was 4 hours.
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Embodiment 2
[0277] To the 48m equipped with two paddle agitators (operated at 270 rpm) and a process control system for regulating process parameters 3 8941.0 kg of 100N oil and 15119.7 kg of a mixture consisting of: methacrylic acid C with a weight ratio of 87.0:13.0 were initially charged into the polymerization reactor of 12 -C 18 Alkyl esters and methyl methacrylate (MMA), along with 25.7 kg of dodecyl mercaptan. The temperature was adjusted to 110°C. Then 39.5 kg of tert-butyl peroctoate were metered in within 3.5 hours, here 6.3% of the total was added in the first 1.5 hours and 10.0% of the total in the next hour and in the following hour 83.7% of the total. The total reaction time was 8 hours.
[0278] ●Molecular weight: 166000g / mol
[0279] ●Polydispersity: 2.41
[0280] ●Kinematic viscosity at 100°C: 1238mm 2 / s
[0281] Thickening (10% of the above product in 150N oil):
[0282] At 100°C: 13.90mm 2 / s
[0283] At 40°C: 75.00mm 2 / s
[0284] ●Viscosity index: 193
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Embodiment 3
[0299] To an 11 m equipped with a MIG stirrer (operating at 31 rpm) and a process control system for regulating process parameters 3 1377.9 kg of 100N oil and 6150.3 kg of a monomer mixture consisting of: methacrylic acid C with a weight ratio of 85.0:15.0 were initially charged into the polymerization reactor of 12-C 18 Alkyl esters and methyl methacrylate (MMA), and 52.3 kg of dodecyl mercaptan. The temperature was adjusted to 110°C. Then 9.8 kg of tert-butyl peroctoate were metered in within 3.5 hours, 6.3% of the total amount in the first 1.5 hours and 10.0% of the total amount in the next hour and 10.0% of the total amount in the last hour. 83.7%. The total reaction time was 8 hours.
[0300] ●Molecular weight: 55400g / mol
[0301] ●Polydispersity: 2.04
[0302] ●Kinematic viscosity at 100°C: 1219mm 2 / s
[0303] Thickening (12% of the above product in 150N oil):
[0304] At 100°C: 10.99mm 2 / s
[0305] At 40°C: 65.3mm 2 / s
[0306] ●Viscosity index: 161
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