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Synthesis method of paracresol-dicyclopentadiene isobutylation resin antioxidant

A technology of dicyclopentadiene isobutyl and p-cresol, which is applied in the synthesis of hindered phenol antioxidants, can solve the problems of difficult removal of catalyst, poor product quality, and poor product chromaticity, and increase the utilization rate of equipment , low ash content and reduced equipment investment

Inactive Publication Date: 2011-02-09
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
Another example is that CN 101402721A discloses a method of p-cresol-dicyclopentadiene isobutylene antioxidant resin, but the quality of the product produced by this method is poor, and the yield is low, and the concentrated sulfuric acid is used in the alkylation process As a catalyst, it is easy to cause emulsification of the product, it is difficult to remove the catalyst, and a large amount of alkali is needed for neutralization, so the product has poor color and high ash content; moreover, concentrated sulfuric acid is highly corrosive, which severely corrodes equipment and requires high equipment, and activated clay is used for decatalysis Decolorization will generate a lot of solid waste and pollute the environment

Method used

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  • Synthesis method of paracresol-dicyclopentadiene isobutylation resin antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a reactor equipped with a stirrer, a reflux condenser, a feeding device and a 250ml nitrogen protection device, add 50g of p-cresol (purity 99.5%), 2g of boron trifluoride complex catalyst, and heat to 60-80 °C, after p-cresol is completely melted, start stirring and raise the temperature to 90-100 °C. At the same time, prepare 30g of dicyclopentadiene, slowly add it into the reactor through the feeding device, after all the dicyclopentadiene is added dropwise, keep the reaction mixture for about 4 hours, control the temperature at 100-105°C, and then lower the temperature to 100°C Below ℃, recover unreacted p-cresol (3.04Kpa, 180℃) under negative pressure, then add toluene and organic composite sulfonic acid catalyst 1.5g to carry out alkylation reaction, feed isobutylene at 75℃ until no absorption stops, add soda ash 1.5g was neutralized, the toluene was recovered by distillation, and the negative pressure (3.0Kpa) was distilled to 240°C to obtain 58g of the produc...

Embodiment 2

[0022] 800 grams of solid p-cresol was charged into a 3000 ml glass kettle, and the air was replaced with nitrogen. Heat up to melting, turn on the stirring blade (rotating speed 60-80 rpm), add 20 grams of condensation catalyst boron trifluoride complex with a dropping funnel, and continue to stir and heat up to 100°C, start adding dicyclopentadiene dropwise 450g. The reaction temperature was controlled at 100±2°C, and the stirring speed was slightly faster during the dropwise addition. After the dropwise addition, keep warm at 100±2°C for 1 hour. Under vacuum (3.04Kpa, 180°C), the moisture, excess p-cresol and small molecular substances were evaporated, and the sampling analysis was completed. Lower the material temperature below 100°C, add toluene (or benzene, or xylene), 40g of organic composite sulfonic acid catalyst and stir, and when the temperature drops to 80±2°C, feed isobutylene to control the reaction temperature. Stop when isobutene is no longer absorbed and in...

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Abstract

The invention relates to a synthesis method of a paracresol-dicyclopentadiene isobutylation resin antioxidant, belonging to the technical field of chemical synthesis. The synthesis method comprises the following steps of: carrying out a condensation reaction on paracresol and dicyclopentadiene to produce phenolic type petroleum resin; then, carrying out an alkylation reaction on the phenolic type petroleum resin and isobutene; and finally, neutralizing by using sodium carbonate, and distilling to obtain the paracresol-dicyclopentadiene isobutylation resin antioxidant. The paracresol-dicyclopentadiene isobutylation resin antioxidant is still prepared by using the paracresol, the dicyclopentadiene and the isobutene as raw materials through the two steps of reactions of condensation and alkylation, but the total yield of the product can reach 93-95% through a special process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing hindered phenol antioxidants. Background technique [0002] At present, there are many kinds of antioxidants used in the technical field of plastics and rubber products, and the typical ones are phenolic and amine antioxidants. Among them, amine antioxidants are mainly used in rubber due to their high toxicity. They are easy to change color during use and have poor compatibility with hydrocarbon oils. The current research direction is phenolic composite antioxidants and polymeric phenols with low toxicity. Antioxidant. Most of the other types have low toxicity. Phenolic antioxidants are the best of all antioxidants and can be divided into monophenolic and bisphenolic antioxidants. Phenolic antioxidants are non-polluting, low-toxic or non-toxic Toxic characteristics, but also has a good antioxidant capacity. [0003] The optimal molecular we...

Claims

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Application Information

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IPC IPC(8): C08G61/02
Inventor 曹宏生吴开运於海霞
Owner JIANGSU FEIYA CHEM IND
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