Method for synthesizing methacryloxyethyl isocyanate
A technology of methacryloyloxyethyl isocyanate and synthesis method, which is applied in the preparation of isocyanate derivatives, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of low product yield, low content, polymerization, carbonization and other problems, to achieve the effect of high product yield and high purity
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Embodiment 1
[0023] (1) Put 500ml of toluene and 61g of ethanolamine (I) (1.0mol) into a 1000ml four-neck flask. While stirring, hydrogen chloride gas was introduced to saturation. Obtain ethanolamine hydrochloride (II) suspension in toluene.
[0024] (2) Add 2 g of 4-dimethylaminopyridine to the ethanolamine hydrochloride (II) toluene suspension prepared above, maintain the temperature at 40°C to 50°C, add 125g of methacryloyl chloride dropwise, and keep warm after dropping React for 2 to 3 hours. After the reaction is over, pass in phosgene at a speed of 1200ml / min to 1400 ml / min. The light passing temperature is 40°C to 50°C. After 2 hours of light passing, the material becomes clear and transparent, and the light passing is stopped. gas. Infuse nitrogen gas to drive away residual phosgene and hydrogen chloride gas to obtain methacryloyloxyethyl isocyanate (MOI) toluene liquid. The content of side reaction 3-chloromethyl-2-methacryloyloxyethyl isocyanate is 0.8%.
[0025] (3) Add 1....
Embodiment 2
[0028] Ethanolamine salt formation is the same as the step (1) of Example 1
[0029] (2) Add 125g of methacryloyl chloride dropwise to the toluene suspension of ethanolamine hydrochloride (II), maintain the dropwise addition temperature at 80°C-85°C, keep the reaction at this temperature for 2-3 hours after dropping, and the reaction is over , and then pass through phosgene at a speed of 1200ml / min to 1400 ml / min, and the light passing temperature is 80°C to 85°C. After 2 hours of light passing, the material becomes clear and transparent, and the passing of phosgene is stopped. Infuse nitrogen gas to drive away residual phosgene and hydrogen chloride gas to obtain methacryloyloxyethyl isocyanate (MOI) toluene liquid. The content of side reaction 3-chloromethyl-2-methacryloyloxyethyl isocyanate is 8.6%.
[0030] The precipitation and rectification are the same as the steps (3) and (4) of Example 1, and the obtained methacryloyloxyethyl isocyanate (MOI) is 127g, the content is ...
Embodiment 3
[0032] Salt formation, condensation, and light passage are the same as steps (1) and (2) of Example 1
[0033] Toluene is removed under reduced pressure and the polymerization inhibitor phenothiazine is not added during rectification. The operation method is the same as the steps (3) and (4) of Example 1, and the obtained methacryloyloxyethyl isocyanate (MOI) is 120g, with a content of 98.5%. , Yield 77.4% (based on ethanolamine, not discounted).
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