Phosphoric acid type trithiocarbonate amphiphilic RAFT (reversible addition-fragmentation chain transfer polymerization) reagent and method for preparing same
A technology of phosphoric acid trithiocarbonate and trithiocarbonate, which is applied in the field of RAFT reagent synthesis, can solve the problems involving the synthesis of phosphoric acid amphiphilic RAFT reagent, etc., and achieve the effect of simple preparation process and widening the scope
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Embodiment 1
[0020] A preparation method of phosphoric acid trithiocarbonate amphiphilic RAFT reagent, comprising the steps of:
[0021] (1) Add 7.3 parts of benzyl mercaptan, 11 parts of 50% sodium hydroxide solution, and 19 parts of deionized water into the reactor at 23°C and nitrogen gas, and react under stirring for 0.5h until the solution is transparent; Add 8.1 parts of carbon disulfide to the transparent solution, and stir for 1.4 hours to obtain trithiocarbonate solution.
[0022] (2) Under ice-bath conditions, add 20 parts of haloalkyl phosphate dropwise to the trithiocarbonate solution in (1) for reaction, and the addition is completed in 0.5 hours; then add 11 parts of 50% sodium hydroxide dropwise Solution, 0.5h dropwise, then add 24 parts of deionized water to dilute, return to 23°C and stir for 24h to obtain phosphoric acid trithiocarbonate solution;
[0023] (3) Under ice-bath conditions, add 48 parts of water to dilute the 4-bromobutylammonium phosphate solution in (2), a...
Embodiment 2
[0025] A preparation method of phosphoric acid trithiocarbonate amphiphilic RAFT reagent, comprising the steps of:
[0026] (1) 9.3 parts of n-butyl mercaptan, 8 parts of 48% potassium hydroxide solution, and 20 parts of deionized water were added to the reactor at 29°C and nitrogen, and the reaction was stirred for 0.5h until the solution was transparent; Add 8.5 parts of carbon disulfide to the above transparent solution, stir and react for 2 hours to obtain trithiocarbonate solution.
[0027] (2) Under ice-bath conditions, add 18 parts of haloalkyl phosphate dropwise to the trithiocarbonate solution in (1) for reaction, and the addition is completed in 0.5 hours; then add 8 parts of 48% potassium hydroxide dropwise The solution was added dropwise for 1 hour, then diluted with 24 parts of deionized water, returned to 29°C and stirred for 23 hours to obtain a phosphoric acid trithiocarbonate solution;
[0028] (3) Under ice-bath conditions, add 40 parts of water to dilute th...
Embodiment 3
[0030] A preparation method of phosphoric acid trithiocarbonate amphiphilic RAFT reagent, comprising the steps of:
[0031] (1) 10 parts of n-propyl mercaptan, 15 parts of 42% sodium hydroxide solution, and 25 parts of deionized water were added to the reactor at 20°C and nitrogen, and the reaction was stirred for 0.8 hours until the solution was transparent; Add 8.6 parts of carbon disulfide to the above transparent solution, stir and react for 1.5 h to obtain trithiocarbonate solution.
[0032] (2) Under ice-bath conditions, add 22 parts of 8-bromooctyl ammonium phosphate dropwise to the trithiocarbonate solution in (1) for reaction, and the dropwise addition is completed in 0.8 h; then add 11 parts of 42 % sodium hydroxide solution, 0.8h dropwise, then add 24 parts of deionized water to dilute, return to 20°C and stir for 14h to obtain phosphoric acid trithiocarbonate solution;
[0033] (3) Under ice bath conditions, add 50 parts of water to dilute the phosphoric acid trit...
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