Process for the preparation of polyalkoxyamines which can be used as initiators for the radical polymerization of polyfunctional living (co)polymers
A polyalkoxyamine and a polymerization reaction technology are applied in the field of preparation of polyalkoxyamines that can be used as initiators for free-radical polymerization of active multifunctional (co)polymers, and can solve the problem that the synthesis of thermal stability is difficult to control. And other issues
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Embodiment 1
[0054] Example 1: Using R 1 =CH 3 , R 2 = H monoalkoxyamine and 1,4-butylene diacrylate to prepare polyalkoxyamine
[0055] A-R in the formula 1 =CH 3 , R 2 Formula (I)-alkoxylamine (2-methyl-2-[N-(tert-butyl)-N-(1-diethoxyphosphoryl-2,2-dimethylpropyl) of =H ) aminooxy] propionic acid) synthesis
[0056]
[0057] Mix 500 ml of degassed toluene, 35.9 g of CuBr (250 mmol), 15.9 g of copper powder (50 mmol) and 86.7 g of N,N,N',N',N"-pentamethyldiethylenetriamine-PMDETA - (500 mmol) was added to a 2-liter glass reactor cleaned with nitrogen, and then at room temperature (20° C.) with stirring, added 500 ml of degassed toluene, 42.1 g of 2-bromo-2-methylpropionic acid (250 mmol) and 78.9 grams of formula
[0058]
[0059] The mixture of nitroxide, which is denoted as SG1, is 84%, ie 225 mmoles.
[0060] The reaction is carried out with stirring at room temperature for 90 minutes, after which the reaction medium is filtered. The filtrate containing toluene was wash...
Embodiment 2
[0090] Embodiment 2: the preparation of linear MMA-BuA-MMA triblock copolymer in solvent medium
[0091] At room temperature, 320 g (ie 2.5 mol) of butyl acrylate and 6.8 g (ie 7.1 mmol) of the polyalkoxyamine prepared in Example 1 were added to a 1 liter jacketed reactor. After degassing several times with nitrogen, the temperature of the reaction medium is raised to 115° C. and this temperature is maintained by thermal regulation for 5 hours. Samples were taken during the reaction for the following purposes:
[0092] - Determination of polymerization kinetics by gravimetric method (measurement of dry extract);
[0093] -Track molecular weight as a function of conversion.
[0094] When the conversion reached 80%, the reaction medium was cooled to 60° C. and residual butyl acrylate was removed by vacuum evaporation.
[0095] At this time, 391 g (ie, 3.7 moles) of methyl methacrylate and 78 g of toluene were added at 60°C. The reaction medium is subsequently heated at 95° C...
Embodiment 3
[0106] Example 3: Preparation of linear MMA-BuA-MMA triblock copolymer in dispersion medium
[0107] The MMA-BuA-MMA triblock copolymer was prepared in three steps:
[0108] First, prepare an organic solution by mixing the following compounds:
[0109] -148 grams (i.e. 1.2 moles) of butyl acrylate,
[0110] - 2.9 g (ie 3.0 mmol) of the polyalkoxyamine prepared in Example 1,
[0111] -0.15 g of polystyrene with a weight average molecular weight (Mw) of 300,000,
[0112] - 1.33 g (ie 5.9 mmol) of hexadecane.
[0113] On the other hand, an aqueous solution is prepared by mixing the following compounds:
[0114] - 595 grams of water,
[0115] - 3.33 grams (i.e. 4.0 mmoles) of Dowfax sold by Dow Chemical Emulsifier (mono- and bis(hexadecyl)disulfonate disodium diphenyl ether)
[0116] -0.64 g (ie 7.6 mmol) NaHCO 3 .
[0117] The two solutions were then mixed for 10 minutes using a magnetic stirrer. This mixture was then subjected to high turbulence for 10 minutes with ve...
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