Preparation method of liquid phosphite antioxidant
A technology of phosphite and triphenyl phosphite, which is applied in the field of antioxidant preparation, can solve the problems of difficult raw material recovery, low raw material utilization rate, long reaction cycle, etc., and achieves easy control of the reaction process and high utilization of raw materials. High efficiency, clear and transparent effect
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Embodiment 1
[0018] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorption device, add 72.79g phenol, 0.7g catalyst 1,8-diazabicycloundec-7-ene, start stirring, control The temperature is 20°C, add 29.51g of phosphorus trichloride dropwise under normal pressure, control the rate of addition, drop it in about 30 minutes, and keep the reaction at 35°C for 2h, then slowly raise the temperature to 150°C, and control the vacuum degree- 0.050MPa, continuously extract the generated HCl gas and absorb it with lye. After the first step reaction is completed, cool down to 40°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst 1,8-diazabicycloundec-7-ene, and raise the temperature to 155±5°C under normal pressure Keep the reaction for 2h, then start to gradually vacuumize to -0.07MPa, and react for 5h. Start distillation after the reaction is completed. The forward distillation is isooctyl alcohol and phenol respectively. Under the condition ...
Embodiment 2
[0020] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorbing device, add 72.79g of phenol and 0.5g of catalyst triethylamine, start stirring, control the temperature at 30°C, and add dropwise 29.51g of triethylamine under normal pressure. Phosphorus chloride, control the dropping rate, drop it in about 45 minutes, keep the reaction at 30°C for 2 hours, then slowly raise the temperature to 150°C, control the vacuum degree -0.070MPa, continuously extract the generated HCl gas, and use lye absorb. After the first step of the reaction, cool down to 40°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst triethylamine, raise the temperature to 155±5°C under normal pressure and keep the reaction for 2h, then start to gradually vacuum to -0.07MPa , Reaction 5h. After the reaction is completed, start distillation. The forward distillation is isooctyl alcohol and phenol respectively. Under the condition of temperature of 185-195...
Embodiment 3
[0022] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorbing device, add 72.79g of phenol, 0.7g of catalyst N,N-dimethylcyclohexylamine, start stirring, control the temperature at 45°C, and Add 29.51g of phosphorus trichloride dropwise under pressure, control the rate of addition, and drop it in about 45 minutes. After the addition is complete, keep the reaction at 40°C for 1h, then slowly raise the temperature to 150°C, control the vacuum degree -0.040MPa, and continuously pump out to form HCl gas, and absorbed with lye. After the first step of the reaction is completed, cool down to 50°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst N,N-dimethylcyclohexylamine, raise the temperature to 160±5°C under normal pressure, keep the reaction for 2h, and then start Gradually evacuate to -0.07MPa, and react for 5h. After the reaction is completed, start distillation. The forward distillation is isooctyl alcohol and phenol ...
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Abstract
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