Comb-type ultra-high molecular weight polymer and synthesis method thereof
A technology of ultra-high molecular weight and synthesis method, applied in the field of comb-type ultra-high molecular weight polymers and synthesis, can solve the problems such as the reports of comb-type alkyl methacrylate or comb-type alkyl acrylate, etc. Intelligent assembly line operation, smooth process, avoid the effect of explosion
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Embodiment 1
[0037] The present embodiment provides a kind of synthetic method of comb type ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0038](1) Preparation of comb-type halide initiator: weigh according to styrene: allyl 2-bromoisobutyrate: allyl isobutyrate: azobisisobutylcyanide mass ratio=100:12:110:0.8 Mix the reagents, add 500g of toluene solvent into a 1000mL reaction bottle, blow nitrogen gas, start stirring, and raise the temperature to 85°C, slowly add the mixed reagents dropwise, after the dropwise addition, keep the reaction at constant temperature for a period of time, spin Steam off the toluene to obtain powdered styrene and 2-bromoallyl isobutyrate copolymer, which is the comb-type halide initiator, and its N=10;
[0039] (2) Preparation of comb-shaped high-molecular-weight polymethyl methacrylate seeds: first take 100 g of methyl methacrylate that has been processed under reduced pressure distillation, and pass through nitrogen...
Embodiment 2
[0042] The present embodiment provides a kind of synthetic method of comb type ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0043] (1) Preparation of the comb-type halide initiator: take by weighing each Mix the reagents, add 500g of toluene solvent into a 1000mL reaction bottle, blow nitrogen gas, start stirring, and raise the temperature to 85°C, slowly add the mixed reagent dropwise, after the dropwise addition, keep the reaction at constant temperature for a period of time, and spin out the toluene , the powdered styrene and 2-bromo allyl propionate copolymer is the comb-type halide initiator, and its N=15;
[0044] (2) Preparation of comb-shaped high-molecular-weight polymethyl methacrylate seeds: first take 100 g of methyl methacrylate that has been processed under reduced pressure distillation, and pass through nitrogen to remove oxygen for later use. In a 1000 mL three-necked reaction flask, add 500 g of ethyl acetate , sti...
Embodiment 3
[0047] The present embodiment provides a kind of synthetic method of comb type ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0048] (1) preparation of comb type halide initiator: with embodiment 1 step (1);
[0049] (2) the preparation of comb type high molecular weight polymethyl methacrylate seed: with embodiment step 1 (2)
[0050] (3) Synthesis of comb-type ultra-high molecular weight polymethyl methacrylate: get 120g comb-type high-molecular-weight polymethyl methacrylate seed solution, wherein, comb-type high-molecular-weight polymethyl methacrylate content is 20g, in nitrogen Under protection, transfer to a 2L reaction kettle with a double planetary mixer, stir with nitrogen, adjust the temperature to 80°C, wait for reflux in the condenser tube, slowly add 1500g of methyl methacrylate monomer dropwise, and the dropping speed is the same as that in the condenser tube It is advisable for the reflux to be stable. While adding d...
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