Method used for one-pot synthesis of p-cresol dicyclopentadiene butylation product

A technology of cresol dicyclopentadiene and dicyclopentadiene, which is applied in the field of synthesizing p-cresol dicyclopentadiene butylated products, can solve the difficulty of increasing post-processing purification, strict reaction conditions, and large safety hazards. problems, to achieve the effect of simple operation, stable reaction system and high safety

Inactive Publication Date: 2017-12-08
广东新华粤石化集团股份公司
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing preparation method of p-cresol dicyclopentadiene butylation product has the following defects: one is to usually use isobutylene, methyl tert-butyl ether and other safe butylation reagents to make butylation The reaction needs to be carried out under the protection of nitrogen, the reaction conditions are strict, and there are great safety hazards; the second is that an additional non-water-soluble solvent needs to be added to the reaction vessel to form a solution system, which increases the difficulty of post-processing purification, and toxic solvents such as toluene and xylene are usually used The 3rd, put into reaction raw material in two steps, need carry out separation and purification to intermediate phenol type petroleum resin, operation is more complicated

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method used for one-pot synthesis of p-cresol dicyclopentadiene butylation product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 148g (2mol) tert-butanol, 27g (0.25mol) p-cresol and 0.54g p-toluenesulfonic acid into a 500mL four-necked reaction flask equipped with a stirrer, a thermometer and a condenser, stir well and slowly heat to 80 After ℃, 20.4g (0.15mol) of dicyclopentadiene was slowly added dropwise for 1 hour, and after the dropwise addition was completed, the reaction was kept at 80℃ for 6 hours. Then, 27 g of sulfuric acid with a mass concentration of 80% was slowly added dropwise into the four-necked reaction flask for 1 hour, and after the dropwise addition was completed, the reaction was kept at 80° C. for 4 hours. After the reaction, the reaction solution in the four-necked reaction flask was left to stand for stratification, and the lower aqueous phase was separated, and the upper organic phase was washed to neutrality with a 5% sodium bicarbonate aqueous solution with a mass concentration, and then the washed liquid Stand for stratification, separate the lower aqueous phase, ...

Embodiment 2

[0036] Add 296g (4mol) tert-butanol, 27g (0.25mol) p-cresol and 1.35g p-toluenesulfonic acid into a 500mL four-necked reaction flask equipped with a stirrer, a thermometer and a condenser, stir well and slowly heat to 70 After ℃, 27.2g (0.2mol) of dicyclopentadiene was slowly added dropwise for 1 hour, and after the dropwise addition was completed, the reaction was kept at 70℃ for 4 hours. Then, the temperature of the reaction liquid in the four-necked reaction flask was lowered to 60°C, and then 5.4g of sulfuric acid with a mass concentration of 93% was slowly added dropwise for 0.2h. After the reaction, the reaction solution in the four-necked reaction flask was left to stand for stratification, and the lower aqueous phase was separated, and the upper organic phase was washed to neutrality with a 5% sodium bicarbonate aqueous solution with a mass concentration, and then the washed liquid Stand for stratification, separate the lower aqueous phase, distill the upper organic ph...

Embodiment 3

[0038] Add 132g (2mol) tert-butanol, 27g (0.25mol) p-cresol and 0.81g p-toluenesulfonic acid to a 500mL four-necked reaction flask equipped with a stirrer, a thermometer and a condenser, stir well and slowly heat to 75 After ℃, slowly add 23.1 g (0.175 mol) of dicyclopentadiene dropwise for 1 hour. After the dropwise addition, keep the reaction at 75 ℃ for 5 hours. Then, the temperature of the reaction liquid in the four-necked reaction flask was lowered to 70°C, and then 13.5g of sulfuric acid with a mass concentration of 85% was slowly added dropwise for 0.4h. After the reaction, the reaction solution in the four-necked reaction flask was left to stand for stratification, and the lower aqueous phase was separated, and the upper organic phase was washed to neutrality with a 5% sodium bicarbonate aqueous solution with a mass concentration, and then the washed liquid Stand for stratification, separate the lower aqueous phase, distill the upper organic phase, recover and remove ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a method used for one-pot synthesis of a p-cresol dicyclopentadiene butylation product. The method comprises following steps: 1, tert-butyl alcohol, p-cresol, and p-toluenesulfonic acid are delivered into a reaction container, an obtained mixture is mixed to be uniform and is heated, dicyclopentadiene is added dropwise for reaction, wherein the molar ratio of p-cresol: dicyclopentadiene: tert-butyl alcohol is controlled to be 1:0.6-0.8:8-16; and 2, sulfuric acid is delivered into the reaction container dropwise for reaction so as to obtain the p-cresol dicyclopentadiene butylation product. The method is high in safety, reaction is easy to control, and operation is simple and convenient.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing p-cresol dicyclopentadiene butylated products in one pot. 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., can prevent the aging of materials and prolong the service life of materials. It is used in the fuel oil industry to inhibit the increase of viscosity and acidity, and it is used in the food and feed industry to prevent food spoilage. [0003] In the prior art, p-cresol dicyclopentadiene butylated products are generally prepared in a two-step process: the first step is to carry out condensation reaction of p-cresol and dicyclopentadiene to generate phenolic petroleum resin; the second step The butylation reaction is carried out between phenol...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02C07C39/17C07C37/14C07C37/11
CPCC08G61/02C07C37/11C07C37/14C08G2261/124C08G2261/1412C08G2261/1422C08G2261/164C08G2261/312C08G2261/3325C07C39/17
Inventor 左洪亮张任熙李红仙刘阳林茂生梁万杰宫召龙
Owner 广东新华粤石化集团股份公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap