A kind of preparation method of bis(2,4-dicumylphenyl) pentaerythritol diphosphite
A technology of pentaerythritol diphosphite and cumylphenyl, which is applied in the field of phosphite antioxidant preparation process, can solve the problems that the product purity is difficult to guarantee, the temperature control requirements are extremely high, and the final use effect of antioxidant 9228 is affected.
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Embodiment 1
[0028] 1) Add 35g of pentaerythritol, 525mg of triethylamine hydrochloride, and 130g of toluene into a reactor equipped with stirring, thermometer, condenser and hydrogen chloride absorption device. Under the condition of mpa, add 74.14g of phosphorus trichloride dropwise for 3.5 hours, then raise the temperature to 45-51°C within 1 hour and keep it for 1 hour, then raise the temperature to 85-90°C within 1.5 hours. °C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction solution;
[0029] 2) Dissolve 175.87g of 2,4-dicumylphenol in 132g of toluene, raise the temperature to 90-100°C, add the dichloropentaerythritol diphosphite reaction solution obtained in step 1) dropwise to 2,4-dicumylphenol In the toluene solution of base phenol, the dropping time is 2 hours, under vacuum gauge pressure-(0.02-0.03)mpa decompression reflux reaction for 4 hours, f...
Embodiment 2
[0032] 1) Add 35g of pentaerythritol, 420mg of di-n-butylamine hydrochloride, and 123g of toluene in a reactor with stirring, thermometer, condenser and hydrogen chloride absorption device, at reaction temperature -5~-2°C, vacuum gauge pressure-( Under the condition of 0.01-0.02mpa), 75.55g of phosphorus trichloride was added dropwise for 3 hours, then the temperature was raised to 45-51°C within 1 hour and kept for 1 hour, and the temperature was raised to 85-90°C within 1 hour. At 85-90 ° C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction liquid;
[0033]2) Dissolve 174.18g of 2,4-dicumylphenol in 148g of toluene, raise the temperature to 90-100°C, add the dichloropentaerythritol diphosphite reaction liquid obtained in step 1) dropwise to 2,4-dicumylphenol In the toluene of base phenol, the dropping time is 1.5 hours, under vacuum gauge press...
Embodiment 3
[0035] 1) Add 70g of pentaerythritol, 1.19g of tri-n-butylamine hydrochloride, and 270g of xylene in a reactor with stirring, thermometer, condenser and hydrogen chloride absorption device, at a reaction temperature of 2-5°C, vacuum gauge pressure-( Under the condition of 0.01-0.02mpa), 149g of phosphorus trichloride was added dropwise for 4 hours, then the temperature was raised to 45-51°C within 1.5 hours and kept for 1 hour, and the temperature was raised to 85-90°C within 1.5 hours. 85-90°C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction liquid;
[0036] 2) Dissolve 355g of 2,4-dicumylphenol in 280g of xylene, raise the temperature to 90-100°C, and add the dichloropentaerythritol diphosphite reaction solution obtained in step 1) dropwise to 2,4-dicumylphenol In the xylene solvent of base phenol, the dropping time is 2.5 hours, under vacuum...
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