Itaconic acid diglycidyl ester, its preparation method and application
A technology of glycidyl ester and itaconic acid two, which is applied to itaconic acid diglycidyl ester and its preparation and application fields, can solve the problem of low epoxy value, and achieve the effects of enriching structure, saving resources and having broad application prospects.
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Embodiment 1
[0037] 1) First mix 100g of itaconic acid and 200g of chloroform evenly, then add 200g of thionyl chloride and 0.5g of N,N'-dimethylformamide, after mixing evenly, under the protection of inert gas, at 50 After reacting at ℃ for 5 hours, the unreacted thionyl chloride and chloroform were distilled off under reduced pressure to obtain itaconic acid chloride;
[0038] 2) Add 500g of chloroform, 100g of pyridine and 100g of 2,3-glycidyl alcohol to the itaconic acid chloride in step 1), react at 0°C for 24 hours under the protection of an inert gas, wash with water, and distill under reduced pressure to remove After solvent and water, diglycidyl itaconate was obtained, the epoxy value was 0.821 (measured by the hydrochloric acid-acetone method), and the viscosity was 0.003 Pa·s. There is 2980cm in the infrared spectrogram of the diglycidyl itaconate prepared by the present embodiment -1 、1710cm -1 、1630cm -1 、1030cm -1and other characteristic absorption peaks; H NMR spectrum s...
Embodiment 2
[0040] 1) Mix 100g itaconic acid, 500g phosgene (at 0°C) and 7g N,N'-dimethylformamide evenly, react at 0°C for 24 hours under the protection of inert gas, and distill under reduced pressure The phosgene of the reaction is obtained itaconic acid chloride;
[0041] 2) Add 400g of toluene, 200g of triethylamine and 200g of 2,3-glycidyl alcohol to the itaconic acid chloride in step 1), react at 30°C for 12 hours under the protection of inert gas, wash with water, and distill under reduced pressure After removing solvent and water, diglycidyl itaconate was obtained, and the epoxy value was 0.825.
[0042] There is 2980cm in the infrared spectrogram of the diglycidyl itaconate prepared by the present embodiment -1 、1710cm -1 、1630cm -1 、1030cm -1 and other characteristic absorption peaks; H NMR spectrum (CD 3 Cl is the solvent), there are characteristic chemical shifts of 6.4ppm, 5.8ppm, 4.4~4.6ppm, 3.9~4.2ppm, 3.2~3.3ppm, 2.5~2.85ppm, of which 6.40ppm and 5.78ppm represent th...
Embodiment 3
[0044] 1) Mix 100g of itaconic acid, 100g of tetrahydrofuran, 300g of oxalyl chloride and 2g of N,N,N′,N′-tetramethylethylenediamine, and react at 30°C for 12 hours under the protection of an inert gas. Pressure distillation removes unreacted oxalyl chloride and tetrahydrofuran to obtain itaconic acid chloride;
[0045] 2) Add 100g of acetone, 100g of xylene, 100g of tetrahydrofuran, 300g of pyridine and 300g of 2,3-glycidyl alcohol, under the protection of an inert gas, react at 50°C for 4 hours, wash with water, and distill off the solvent and water under reduced pressure to obtain Diglycidyl itaconate, the epoxy value is 0.819.
[0046] There is 2980cm in the infrared spectrogram of the diglycidyl itaconate prepared by the present embodiment -1 、1710cm -1 、1630cm -1 、1030cm -1 and other characteristic absorption peaks; H NMR spectrum (CD 3 Cl is the solvent), there are characteristic chemical shifts of 6.4ppm, 5.8ppm, 4.4~4.6ppm, 3.9~4.2ppm, 3.2~3.3ppm, 2.5~2.85ppm, of...
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