Linear controllable ultra-high molecular weight polyalkyl methacrylate and synthesis method
A polyalkyl methacrylate, ultra-high molecular weight technology, applied in the polymer field, can solve problems such as difficulty in realizing large-scale industrial production and limited molecular growth with the increase of solid content, so as to improve the molecular weight of polymers, Good heat dissipation effect, ensure the effect of heat dissipation effect
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Embodiment 1
[0045] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0046] (1) Preparation of high-molecular-weight polymethyl methacrylate seeds: first take 100 g of methyl methacrylate that has been processed by vacuum distillation, and pass nitrogen to remove oxygen for later use. In a 1000 ml three-necked reaction flask, add 500 g of ethyl acetate, and pass nitrogen Stir, add 0.05g ethyl 2-bromoisobutyrate, 0.03g copper powder, 0.03g cuprous bromide, 0.05g pentamethyldiethylenetriamine, 0.005g disodium edetate, and mix well , raise the temperature to 50°C, add 10g of methyl methacrylate at one time until the system becomes slightly viscous, then adjust the temperature to 78°C, ethyl acetate refluxes in the condenser, slowly add the remaining 90g of methacrylic acid dropwise Methyl ester, the rate of addition is based on the reflux state. After the addition is completed, react at a constant ...
Embodiment 2
[0049] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0050] (1) preparation of high molecular weight polymethyl methacrylate seed: with embodiment 1 step (1);
[0051] (2) Synthesis of ultra-high molecular weight polymethyl methacrylate: Methyl methacrylate is processed through vacuum distillation, feed nitrogen deoxygenation for subsequent use, get the high molecular weight polymethyl methacrylate prepared by 120g step (1) Seed solution, wherein the high molecular weight polymethyl methacrylate seed content is 20g, under the protection of nitrogen, transfer to a 2L reaction kettle with a double planetary mixer, stir with nitrogen, raise the temperature to 78 ° C, and wait for the condensation tube reflux in the medium, slowly add 750g of spare methyl methacrylate monomer dropwise, the rate of addition should be stable with the reflux in the condenser tube, after the 750g methyl ...
Embodiment 3
[0053] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:
[0054] (1) preparation of high molecular weight polymethyl methacrylate seed: with embodiment 1 step (1);
[0055] (2) Synthesis of ultra-high molecular weight polymethyl methacrylate: Methyl methacrylate is processed through vacuum distillation, feed nitrogen deoxygenation for subsequent use, get the high molecular weight polymethyl methacrylate prepared by 120g step (1) Seed solution, wherein the high molecular weight polymethyl methacrylate seed content is 20g, under the protection of nitrogen, transfer to a 2L reaction kettle with a double planetary mixer, stir with nitrogen, raise the temperature to 85 ° C, wait for the condensation tube Backflow occurs in the middle, slowly add 1500g methyl methacrylate monomer dropwise, the rate of addition should be stable with the reflux in the condenser tube, after the 750g methyl met...
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