Synthesis method of 1,4-butylene glycol dimethacrylate
A technology of dimethyl benzoate and synthesis method, applied in the synthesis of 1,4-butanediol dimethacrylate, in the field of 1,4-butanediol dimethacrylate, can solve the loss of raw materials Large size, complex process, serious equipment corrosion, etc., to achieve the effect of mild reaction conditions, simple post-processing, and low environmental pollution
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Embodiment 1
[0019] A kind of synthetic method of 1,4-butanediol dimethacrylate, at room temperature the methacrylic acid of 69.54g, the 1,4-butanediol of 28g, the stopper hydroquinone of 0.49g and Put 29.26g of cyclohexane with water agent into a three-necked flask equipped with a water separator, reflux condenser, stirrer and thermometer, dissolve and stir evenly, then heat up to 85°C, add 0.49g of HZSM-5 molecular sieve catalyst, and then Heat up and maintain at 100°C, continue the reaction until no water comes out from the water separator, and end the reaction. It takes 4 hours, and the acid value of the test reaction system is 0.048mgKOH / g. The catalyst was separated by filtration, and the light yellow organic phase was separated with a separatory funnel, and the organic phase was washed with distilled water for 3 times, then the temperature was raised to 70°C, and the organic solvent was distilled off under reduced pressure under a pressure of 0.03-0.04 MPa, cooled Finally, the targe...
Embodiment 2
[0021] Put methacrylic acid 74.89g, 1,4-butanediol 28g, polymerization inhibitor hydroquinone 0.67g and water-carrying agent cyclohexane 36.01g into the reaction bottle equipped with a water separator, stir and dissolve, and heat up to 80°C, add 1.03g of HZSM-5 molecular sieve catalyst, then heat up and maintain at 105°C, 1,4-butanediol reacts with methacrylate to generate 1,4-butanediol dimethyl benzoate , continue to react until there is no water out of the water separator, and the reaction is ended. It takes 3.5 hours, and the acid value of the reaction is measured to be 0.054mgKOH / g. The catalyst was separated by filtration, the separatory funnel stood still to separate the light yellow organic phase, and the organic phase was washed twice with distilled water, then the temperature was raised to 80°C, and the organic solvent was distilled off under reduced pressure under a pressure of 0.05-0.06 MPa. After cooling, The target product 1,4-butanediol dimethacrylate was obtain...
Embodiment 3
[0023] Put 80.24g of methacrylic acid, 28g of 1,4-butanediol, 0.87g of inhibitor hydroquinone and 43.3g of water-carrying agent cyclohexane into the reaction bottle equipped with a water separator, stir and dissolve, and heat up to At 90°C, add 1.08g of HZSM-5 molecular sieve catalyst, then heat up and maintain at 110°C to continue the reaction, 1,4-butanediol reacts with methacrylate to generate 1,4-butanediol dimethylbenzene Ester, react until there is no water coming out of the water separator, then the reaction ends, and it takes 3 hours, and the acid value of the reaction is measured to be 0.034mgKOH / g. The catalyst was separated by filtration, the separatory funnel stood still to separate the light yellow organic phase, and then the organic phase was washed with distilled water for 3 times, then the temperature was raised to 70-75°C, and the organic solvent was distilled off under reduced pressure under a pressure of 0.04-0.05MPa. After cooling, the target product 1,4-bu...
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