Preparation technique of high-purity hydroxyethyl methacrylate
The technology of hydroxyethyl methacrylate and methacrylic acid is applied in the field of preparation technology of hydroxy methacrylate, which can solve the problems of difficult handling of polymers and easy occurrence of polymerization reaction, so as to improve the polymerization inhibition effect and prevent the polymerization reaction. , to prevent the effect of violent aggregation
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[0028] Example 1:
[0029] Under vacuum conditions, 2000kg of methacrylic acid, 2.0% chromium acetate, 13×10 -4 After the completion of the hydroquinone and p-hydroxyanisole, ensure that the vacuum is 0.75Mpa. After nitrogen replacement, add ethylene oxide to the measuring tank to ensure that the oxygen / nitrogen volume ratio is 0.25%. The steam is heated to 80°C. Add ethylene oxide, control the dropping rate of ethylene oxide to ensure that the pressure is less than or equal to 60KPa, the molar ratio of ethylene oxide to methacrylic acid is 1.02:1, and the reaction temperature is controlled at 90℃ by cooling water and the reaction time is 1.5 hours. ; After the dripping is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, the addition reaction is deemed to be completed by sampling and testing the mass percentage of methacrylic acid to be less than 0.5%;
[0030] Under vacuum conditions, a thin film evaporator is used for de...
Example Embodiment
[0034] Example 2:
[0035] Under vacuum conditions, 2000kg of methacrylic acid, 5.0% chromium acetate, 13×10 -4 Hydroquinone and p-hydroxyanisole and 5×10 -3 After the completion of the water, ensure that the vacuum is at 0.75Mpa, fill with nitrogen to ensure the oxygen / nitrogen volume ratio is 0.25%, and add ethylene oxide dropwise when the steam is heated to 80°C, and ensure that the pressure is ≤60KPa by controlling the dropping rate of ethylene oxide , The molar ratio of ethylene oxide to methacrylic acid is 1.06:1, the reaction temperature is controlled at 90℃ by cooling water, and the reaction time is 1.5 hours; after the dripping is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, samples are taken to detect methyl The mass percentage of acrylic acid is less than 0.5% as the addition reaction is complete;
[0036] Under vacuum conditions, a thin film evaporator is used for deweighting to obtain a primary distillatio...
Example Embodiment
[0037] Example 3:
[0038] Under vacuum conditions, 2000kg of methacrylic acid, 2.0% chromium acetate, 13×10 -4 Hydroquinone and p-hydroxyanisole and 5×10 -3 After the completion, ensure that the vacuum is at 0.75Mpa, fill with nitrogen to ensure that the oxygen / nitrogen volume ratio is 0.25%, and add ethylene oxide dropwise when the steam is heated to 85℃, and ensure that the pressure is ≤60KPa by controlling the dropping rate of ethylene oxide , The molar ratio of ethylene oxide to methacrylic acid is 1.02:1, and the reaction temperature is controlled at 90℃ by cooling water, and the reaction time is 1.5 hours; after the addition is completed, the cooling water is turned off and the temperature rises naturally. After the temperature drops, samples are taken to detect methyl The mass percentage of acrylic acid is less than 0.5% as the addition reaction is complete;
[0039] Under vacuum conditions, a thin film evaporator is used for deweighting to obtain a primary distillation pro...
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