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Method for preparing p-cresol dicyclopentadiene butylation product

A technology of cresol dicyclopentadiene and dicyclopentadiene, which is applied in the field of preparing p-cresol dicyclopentadiene butylated products, can solve the problems of low safety, achieve recycling, easy separation, and avoid toxicity The effect of the solvent

Active Publication Date: 2017-05-10
广东希必达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, isobutylene and tert-butyl methyl ether are butylation raw materials with low safety

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] The method for preparing p-cresol dicyclopentadiene butylated product of the present invention mainly comprises: after weighing tert-butanol and p-cresol-dicyclopentadiene resin in proportion and mixing, heating and mixing evenly, and reacting under the action of a strong acid catalyst . After the reaction, the catalyst was separated and removed and washed until neutral, and the organic phase was distilled off to obtain a light yellow solid product p-cresol dicyclopentadiene butylated product. Using tert-butanol with higher safety as the raw material for butylation reaction is safe in operation and greatly avoids potential safety hazards.

[0014] The molar ratio of the tert-butanol to p-cresol-dicyclopentadiene resin is 4:1˜50:1, preferably 8:1˜20:1. Excess tert-butanol is used as a reaction solvent, and the reaction raw materials are simple and convenient to control the reaction, and other toxic solvents such as toluene (or xylene) are avoided. Excess tert-butanol c...

Embodiment 1

[0022] Add 296g (4mol) tert-butanol and 269g (0.5mol) p-cresol-dicyclopentadiene resin (average molecular weight: 538) into a 1000mL four-necked reaction flask equipped with stirring, thermometer and condenser and heat to 80°C Mix tert-butanol and p-cresol-dicyclopentadiene resin evenly, then lower the temperature to 65-70°C, slowly add 148g of sulfuric acid (the mass concentration of sulfuric acid is 80%) dropwise, finish adding sulfuric acid in 1 hour, and keep warm for 4 hours after adding. After the reaction was completed, the layers were left to stand, the catalyst sulfuric acid in the lower layer was separated off, and the organic phase in the upper layer was washed with 5% aqueous sodium bicarbonate until neutral. Then the organic phase was distilled to recover and remove excess tert-butanol to obtain a light yellow solid product p-cresol dicyclopentadiene butylated product with a product weight of 320 g and a yield of 98.5%. The butylation rate was analyzed by HPLC to ...

Embodiment 2

[0024] In a 1000mL four-necked reaction flask equipped with stirring, thermometer and condenser, add 390g (5mol) tert-butanol, 134.5g (0.25mol) p-cresol-dicyclopentadiene resin (average molecular weight is 538) and heat to 80 ℃ to mix tert-butanol and p-cresol-dicyclopentadiene resin evenly, then lower the temperature to 30-35 ℃, slowly add 78g of sulfuric acid (the mass concentration of sulfuric acid is 93%) dropwise, and finish adding for 1h. After adding, keep warm for 8h. After the reaction was completed, the layers were left to stand, the catalyst sulfuric acid in the lower layer was separated, and the organic phase in the upper layer was washed with 5% aqueous sodium bicarbonate until neutral. Then the organic phase was distilled to recover and remove excess tert-butanol to obtain a light yellow solid product p-cresol dicyclopentadiene butylated product, the product weight was 159 g, the yield was 97.8%, and the butylation rate was 99.0% according to HPLC analysis.

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Abstract

The invention discloses a method for preparing a p-cresol dicyclopentadiene butylation product. After tert butyl alcohol and p-cresol-dicyclopentadiene are weighed in proportion, then even heating and mixing are performed, and a strong acid catalyst is added for reaction; after reaction is completed, a catalyst is removed through separation, washing is performed to reach a neutral state, an organic phase is removed through distillation, and the a p-cresol dicyclopentadiene butylation product is obtained, wherein the male ratio of the tert butyl alcohol to p-cresol dicyclopentadiene resin is 4:1 to 50:1, the reaction temperature is 20-83 DEG C, and the reaction time is 2-12 hours. The method for preparing the p-cresol dicyclopentadiene butylation product adopts the tert butyl alcohol high in safety as a raw material to perform butylation reaction, and potential safety hazards caused by usage of butylation raw materials such as isobutene and tert-butyl methyl ether low in safety are avoided.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing p-cresol dicyclopentadiene butylated product. Background technique [0002] P-cresol dicyclopentadiene butylated product antioxidant is one of the few non-toxic, odorless and light-colored antioxidants among phenolic antioxidants. It is widely used in rubber, plastic, fiber , adhesives, etc., to prevent the aging of materials and prolong the service life of materials. It is also used to inhibit the increase of viscosity and acidity in the fuel oil industry, and to prevent food spoilage in the food and feed industry. [0003] P-cresol dicyclopentadiene butylation product Antioxidant products are usually made of p-cresol as the main raw material, and react with dicyclopentadiene to form phenolic petroleum resin, and then carry out alkylation reaction with isobutylene. . For example, the condensation reaction of methylphenol and dicyclopentadiene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/16C07C39/17
CPCC07C37/16C07C39/17
Inventor 左洪亮刘阳庞海舰张任熙李红仙宫召龙
Owner 广东希必达新材料科技有限公司
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