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Method for producing aggregate-type hindered phenol antioxidant

A hindered phenol antioxidant, polymerization type technology, applied in the field of chemical synthesis, can solve problems such as cumbersome process, achieve the effects of clean and environmentally friendly process, low ash content, and simple treatment process

Inactive Publication Date: 2013-09-25
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a large amount of cyclohexane solvent in the reaction process, and decolorizes with activated carbon in the post-treatment, and the process is cumbersome

Method used

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  • Method for producing aggregate-type hindered phenol antioxidant
  • Method for producing aggregate-type hindered phenol antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under the protection of nitrogen, add 132Kg xylene and 162Kg (1.5Kmol) p-cresol into the 1500L enamel reaction kettle, stir and raise the temperature to 140°C to remove the water in the solution. Then lower the temperature to 80° C. and add 1.32 kg of organic composite sulfonic acid catalyst dropwise. After stirring evenly, add 132Kg (1 Kmol) of dicyclopentadiene dropwise for 3 hours. After the dropwise addition was completed, the temperature was continued to rise to 150°C for 9 hours. The temperature of the reaction feed liquid was lowered to 50°C, and 132Kg (1.5Kmol) tert-butyl methyl ether was added dropwise for 2 hours. After the dropwise addition, the temperature was raised to 150° C. to continue the reaction for 9 h.

[0028] After the reaction was completed, the temperature was lowered to room temperature. Then add 100Kg saturated brine to the reaction kettle to wash twice, stir, and let stand to separate layers. Then wash the organic layer with 100Kg 5% sodi...

Embodiment 2

[0030] Under the protection of nitrogen, add 660Kg toluene and 162Kg (1.5Kmol) p-cresol into the 2000L enamel reaction kettle, stir and raise the temperature to 140°C to remove the water in the solution. Then lower the temperature to 80° C. and add 132 Kg of organic composite sulfonic acid catalyst dropwise. After stirring evenly, add 132Kg (1Kmol) of dicyclopentadiene dropwise for 3 hours. After the dropwise addition was completed, the temperature was continued to rise to 150°C for 9 hours of reaction. The temperature of the reaction feed liquid was lowered to 50°C, and 132Kg (1.5Kmol) tert-butyl methyl ether was added dropwise for 2 hours. After the dropwise addition was completed, the temperature was raised to 150° C. to continue the reaction for 9 h.

[0031] After the reaction was completed, the temperature was lowered to room temperature. Then add 100Kg saturated brine to the reaction kettle to wash twice, stir, and let stand to separate layers. Then wash the organic...

Embodiment 3

[0033] Under the protection of nitrogen, add 660Kg chlorobenzene and 216Kg (2Kmol) p-cresol into the 1500L enamel reaction kettle, stir and raise the temperature to 140°C to remove the water in the solution. Then lower the temperature to 80° C. and add 1.32 kg of organic composite sulfonic acid catalyst dropwise. After stirring evenly, add 132Kg (1Kmol) of dicyclopentadiene dropwise for 3 hours. After the dropwise addition was completed, the temperature was continued to rise to 150°C for 9 hours of reaction. The temperature of the reaction feed liquid was lowered to 50°C, and 176Kg (2Kmol) of tert-butyl methyl ether was added dropwise for 2 hours. After the dropwise addition was completed, the temperature was continued to rise to 150° C. for 9 h.

[0034] After the reaction was completed, the temperature was lowered to room temperature. Then add 100Kg saturated brine to the reaction kettle to wash twice, stir, and let stand to separate layers. Then wash the organic layer w...

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Abstract

The invention provides a method for producing aggregate-type hindered phenol antioxidant. The method comprises the following steps of: firstly reacting p-cresol with dicyclopentadiene and a non-water-solubility solvent through an organic composite sulfonic acid catalyst under the anhydrous condition to obtain p-cresol-dicyclopentadiene resin; then adding tert-Butyl methyl ether so as to produce a p-cresol-dicyclopentadiene-isobutylated resin crude product, or firstly reacting the p-cresol with the tert-Butyl methyl ether and the non-water-solubility solvent through the organic composite sulfonic acid catalyst under the anhydrous condition to obtain an o-tert-butyl p-cresol; then adding the dicyclopentadiene so as to produce the p-cresol-dicyclopentadiene-isobutylated resin crude product; washing the crude product by water, and carrying out steam distillation on the crude product to obtain the aggregate-type hindered phenol antioxidant, wherein the final yield reaches more than 95%. The method has the advantages that the adopted organic composite sulfonic acid catalyst is low in cost, common and easy to wash by water and separate, water can be recycled, the product has good color and luster, low ash content and high purity, the treatment process is simple, equipment is free of being corroded, the technology is clean and environmentally-friendly, and the product yield reaches more than 95%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for producing p-cresol-dicyclopentadiene-isobutylated resin through a one-pot method of polymerizing hindered phenol antioxidant. Background technique [0002] p-cresol-dicyclopentadiene-isobutylated resin (antioxidant CPL) is a new type of high-efficiency and non-discoloring steric hindered polymerization phenolic antioxidant. Due to its moderate molecular weight, it has heat resistance, The characteristics of good compatibility between anti-extraction and resin are in line with the current development trend of polymer antioxidants towards high efficiency, non-toxicity, heat resistance, anti-extraction and anti-discoloration. [0003] P-cresol-dicyclopentadiene-isobutylated resin antioxidant products usually use p-cresol as the main raw material, undergo condensation reaction with dicyclopentadiene to produce phenolic petroleum resin, and then carry out alkylat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/17C07C37/11C07C37/14C08K5/13
Inventor 徐保明唐强陈坤裴智山杨添李洁刘莹韩洋洋张杰胡欢
Owner HUBEI UNIV OF TECH
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