Method for separating triisobutylene in tert-butyl acrylate reaction liquid
A technology of triisobutyl acrylate and tert-butyl acrylate, which is applied in the field of separation of triisobutylene in tert-butyl acrylate reaction solution, can solve the problem of unqualified recycled acrylic acid, and achieve the effect of solving unqualified
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Embodiment 1
[0066] 1) Add sodium p-vinylphenolate to N,N dimethylformamide, stir evenly, add tetrabutylammonium bromide, and then add ClCF 2 Cl, of which sodium vinylphenolate and ClCF 2 The molar ratio of Cl is 1:3, and the catalyst is sodium vinylphenate and ClCF 2 1 wt% of the Cl weight sum, reacted at 30°C for 4 hours, extracted and purified, and obtained the fluoride of styrene;
[0067] 2) Mix vinyltrimethoxysilane, styrene fluoride, tetrafluoroethylene, 1,4-butanediol diacrylate, decane, and azobisisobutyronitrile in a molar ratio of 1:1:0.2: 0.05:0.2:0.01 for feeding, using suspension polymerization at 80°C to prepare polymer microspheres;
[0068] 3) Swell the polymer microspheres in methanol for 4 hours, then add concentrated sulfuric acid with a molar ratio of 1:0.5, perform sulfonation reaction at 40°C for 5 hours, filter and wash with water to obtain 1# solid superacid;
[0069] 4) 1# solid superacid is analyzed by BET specific surface area detection method, and its specif...
Embodiment 2
[0071] 1) Add potassium p-vinylphenate to N,N dimethylacetamide, stir evenly, add tetrabutylammonium iodide, and then add Br(CF 2 ) 6 Br, where potassium vinylphenate and Br(CF 2 ) 6 The molar ratio of Br is 1:2, and the catalyst is potassium vinylphenate and Br(CF 2 ) 6 0.5wt% of the weight sum of Br, finally reacted at 10°C for 6 hours, extracted and purified, and obtained fluoride of styrene;
[0072] 2) Vinyl triethoxysilane, styrene fluoride, tetrafluoroethylene, 1,6-hexanediol diacrylate, n-undecane, and ammonium persulfate in a molar ratio of 1:0.2:5: 0.5:2.0:0.02 for feeding, using suspension polymerization at 100°C to prepare polymer microspheres;
[0073] 3) Swell the polymer microspheres in ethanol for 3 hours, then add chlorosulfonic acid with a molar ratio of 1:5, perform a sulfonation reaction at 100°C for 5 hours, filter and wash with water to obtain 2# solid superacid;
[0074] 4) 2# solid superacid is analyzed by BET specific surface area detection metho...
Embodiment 3
[0076] 1) Add sodium p-vinylphenolate in dichloromethane, stir well and add tetrabutylammonium bromide, then add I(CF 2 ) 3 I, where sodium vinylphenolate and I(CF 2 ) 3 The molar ratio of I is 1:3, and the catalyst is sodium vinylphenate and I(CF 2 ) 3 3wt% of 1 weight and 3wt%, finally reacted between 50 ℃ for 2 hours, extracted and purified, obtained the fluoride of styrene;
[0077] 2) Vinyl triphenoxysilane, styrene fluoride, tetrafluoroethylene, 1,6 hexanediol dimethacrylate, n-eicosane, and potassium persulfate in a molar ratio of 1:0.2:2 : 0.1:1:0.01 for feeding, using suspension polymerization at 85°C to prepare polymer microspheres;
[0078] 3) Swell the polymer microspheres in ether for 6 hours, then add sodium sulfite with a molar ratio of 1:3, perform sulfonation reaction at 70°C for 7 hours, filter and wash with water to obtain 3# solid superacid;
[0079] 4) 3# solid superacid is analyzed by BET specific surface area detection method, and its specific surf...
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