Azidization copolymer modified graphite modified polystyrene-based resin preparation method
A nitriding copolymer and polystyrene-based technology, which is applied in the field of preparation of azidated copolymer-modified graphite-modified polystyrene-based resin, can solve the problems of ozone depletion, high product cost, and low solubility, and achieve improved Thermal insulation performance, stable product performance, and the effect of improving solubility
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[0021] A method for preparing azide copolymer modified graphite-modified polystyrene-based resin of the present invention is characterized in that it comprises the following steps.
[0022] a) Styrene pretreatment: wash with 5% sodium hydroxide solution for 3-5 times, wash with deionized water until the pH is about 7, remove water from calcium hydride and distill under reduced pressure.
[0023] b) Surface modification of graphite: After mixing acryloyl chloride, methyl styrene and brominated styrene in a certain proportion, add an initiator and react at 60-100°C for 3-24 hours. Dissolve the prepared copolymer in tetrahydrofuran, react with an aqueous azide solution at -10~5°C for 5~20h to obtain an azide copolymer, add the azide copolymer and graphite to N,N-di Stirring in methyl acetamide solvent at 140-160°C for 1-8 hours to prepare azide-copolymer-modified graphite.
[0024] c) Preparation of styrene-based resin: react the modified graphite, styrene monomer and methacryla...
Embodiment 1
[0033] a) Styrene pretreatment: wash 3 times with 5% sodium hydroxide solution by mass, wash with deionized water until the pH is around 7, remove water with calcium hydride and distill under reduced pressure.
[0034] b) React 300 g of acryloyl chloride, 375 g of methyl styrene, 75 g of brominated styrene, and 2 g of azobisisobutyronitrile at 70° C. for 3 h to prepare a copolymer. Dissolve 600g of the prepared copolymer in 1000ml of tetrahydrofuran, react with 300ml of 30% sodium azide aqueous solution at -8°C for 12h, and remove the solvent to obtain an azide copolymer. Dissolve 500 g of azide copolymer in 800 ml of N,N-dimethylacetamide solvent, add 50 g of graphite and stir at 149° C. for 3 h, remove the solvent, and obtain azide copolymerized modified graphite.
[0035] c) Add 50g of the modified graphite prepared in step b), 9.0kg of styrene monomer (removing the polymerization inhibitor), 0.94kg of methyl methacrylate, and 10g of azobisisobutyronitrile into the reaction...
Embodiment 2
[0039] a) Styrene pretreatment: wash 3 times with 5% sodium hydroxide solution by mass, wash with deionized water until the pH is around 7, remove water with calcium hydride and distill under reduced pressure.
[0040] b) React 150 g of acryloyl chloride, 150 g of methyl styrene, 75 g of brominated styrene, and 2 g of azobisisobutyronitrile at 60° C. for 15 h to prepare a copolymer. Dissolve 250 g of the prepared copolymer in 200 ml of tetrahydrofuran, react with 400 ml of a 25% sodium azide aqueous solution at -10°C for 18 hours, and remove the solvent to obtain an azide copolymer. Dissolve 250g of azidated copolymer in 200ml of N,N-dimethylacetamide solvent, add 100g of graphite and stir at 140°C for 8h, remove the solvent, and obtain azidized copolymerized modified graphite.
[0041] c) Add 150g of the modified graphite prepared in step b), 7kg of styrene monomer, 3kg of ethyl methacrylate, and 10g of azobisisobutyronitrile into the reaction kettle, and stir at 145°C for 2h...
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