Preparation method of liquid hindered phenol carboxylic ester antioxidant
A phenol carboxylate and antioxidant technology, which is applied in the field of preparation of liquid antioxidants, can solve the problems of complex post-treatment process, loss of raw material alcohol, environmental problems, etc., and achieves simplified product post-treatment process, reduced reaction time, The effect of avoiding environmental problems
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[0017] The preparation method of the solid base catalyst is as follows: uniformly mix magnesium oxide powder and NaY zeolite in a predetermined ratio, irradiate at a microwave frequency of 1000-3000 MHz for 10-60 minutes, and then activate at 180-300 ° C, and the activation time is preferably 1-5 minutes. hours, a solid base catalyst was obtained.
[0018] The solid base catalyst can continue to be used after being regenerated. The regeneration method is to wash the reacted catalyst with ethanol, filter it, and then activate it at 180-300° C., and the activation time is preferably 1-5 hours.
[0019] The present invention will be described in detail below by examples, but the present invention is not limited thereto.
example 1
[0021] Weigh 160g of decanol, 7g of KOH and 0.6g of nickel powder into a 250ml three-necked reaction bottle with stirring and water separator, stir well and heat up to 230°C, during the reaction process, the water produced by the reaction is continuously removed by the water separator The reaction system was separated, the reaction was carried out for 60 minutes, and the reaction was terminated. After the reactant was cooled, it was filtered. The filtrate is distilled under reduced pressure to obtain C with a purity of more than 95% by mass. 20 Guerbert ol.
[0022] The magnesium oxide powder and NaY zeolite were uniformly mixed at a mass ratio of 1:5.7, irradiated at a microwave frequency of 2000MHz for 30min, and then activated at 200°C for 3 hours to obtain a solid base catalyst A, wherein the MgO content was 15% by mass.
[0023] 149g (0.5mol) C 20 Grignard alcohol, 146g (0.5 mole) (3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate and 1.25g solid base catalyst A wer...
example 2
[0026] Weigh 160g of octanol, 7g of KOH and 0.4g of nickel powder into a 250ml three-necked reaction bottle with stirring and water separator, stir well and raise the temperature to 220°C. The reaction system was separated, the reaction was carried out for 50 minutes, and the reaction was terminated. After the reactant was cooled, it was filtered. The filtrate is subjected to vacuum distillation to obtain C with a purity of more than 95% by mass. 16 Guerbert ol.
[0027] The magnesium oxide powder and NaY zeolite were uniformly mixed at a mass ratio of 1:11.5, irradiated at a microwave frequency of 1200MHz for 20min, and then activated at 180°C for 2 hours to obtain a solid base catalyst B, wherein the MgO content was 8% by mass.
[0028] 121g (0.5mol) C 16 Grignard alcohol, 146g (0.5 mole) (3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate and 1.5g solid base catalyst B were added to the reaction system with a water separator, stirred and heated . Under the protection...
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