Check patentability & draft patents in minutes with Patsnap Eureka AI!

High-yield green and safe synthesis method of 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride

A technology of biphenyltetracarboxylic dianhydride and biphenyltetracarboxylic acid, which is applied in the field of synthesis of acid anhydride raw material monomers of polyimide, can solve the problems of high cost, low synthesis technology yield, non-green environmental protection and the like, and achieves low pollution. , high yield, the effect of reducing production costs

Active Publication Date: 2021-11-30
JIANGXI NORMAL UNIV
View PDF11 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the technical deficiencies in the prior art, such as low yield, non-environmental protection, and high cost of the synthesis technology, the present invention provides a high-yield, environmentally friendly and low-cost synthetic methods

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
  • High-yield green and safe synthesis method of 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride
  • High-yield green and safe synthesis method of 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride
  • High-yield green and safe synthesis method of 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] This example provides a high-yield green and safe synthesis method of 3,3',4,4'-biphenyltetracarboxylic dianhydride, the reaction equation of which is as follows:

[0033]

[0034] This synthetic method comprises the steps:

[0035] Add 400.0g of distilled water in the four-necked flask equipped with thermometer, stirrer, air duct and reflux device, add 27g of sodium hydroxide (0.675mol) under stirring, add 50g of 4-chlorophthalic anhydride (0.275mol) after dissolving ), stirred at room temperature for 1 hour, then added 0.3g of 10wt%Pd / C (with 0.5% concentration of glucose aqueous solution in 300 ℃ of nitrogen atmosphere to do the anhydrous palladium carbon of carbonization bonding treatment), 20g composite reducing agent (β-cyclodextrin / serine / xylitol=5 / 3 / 2), bubbling with nitrogen for 30min, then heating up to 95°C under nitrogen protection, reacting for 10h, cooling to room temperature, filtering, drying and drying under nitrogen protection Reclaim palladium-car...

Embodiment 2

[0037] This example provides a high-yield green and safe synthesis method of 3,3',4,4'-biphenyltetracarboxylic dianhydride, the reaction equation of which is as follows:

[0038]

[0039] This synthetic method comprises the steps:

[0040] Add 400.0g of distilled water in the four-necked flask equipped with thermometer, stirrer, air duct and reflux device, add 27g of sodium hydroxide (0.675mol) under stirring, add 50g of 4-chlorophthalic anhydride (0.275mol) after dissolving ), stirred at room temperature for 1 hour, then added 0.306g of reclaimed 10%Pd / C from Example 1, 20g composite reducing agent (β-cyclodextrin / serine / xylitol=5 / 3 / 2) , nitrogen bubbling for 30min, then heated up to 95°C under nitrogen protection, reacted for 10h, cooled to room temperature and filtered, dried under nitrogen protection and recovered palladium carbon catalyst 0.305g (recovery rate 102%); 20% was added dropwise to the filtrate Concentrated hydrochloric acid to adjust the acidity to PH = 3;...

Embodiment 3

[0042] This example provides a high-yield green and safe synthesis method of 3,3',4,4'-biphenyltetracarboxylic dianhydride, the reaction equation of which is as follows:

[0043]

[0044] This synthetic method comprises the steps:

[0045] Add 400.0 g of distilled water to a four-neck flask equipped with a thermometer, a stirrer, an air duct and a reflux device, add 27 g of sodium hydroxide (0.675 mol) under stirring, and add 50 g of 4-chlorophthalic anhydride (0.275 mol) after dissolving , stirred at room temperature for 1 hour, then added 0.305g of 10wt% Pd / C recovered from Example 2, 40g composite reducing agent (-cyclodextrin / serine / xylitol=5 / 3 / 2), Nitrogen was bubbled for 30 min, then the temperature was raised to 95° C. under the protection of nitrogen, reacted for 10 h, cooled to room temperature and filtered, dried and recovered palladium carbon catalyst 0.304 g (recovery rate 101.3%) under the protection of nitrogen; Adjust the acidity with hydrochloric acid to PH...

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 the technical field of synthesis of anhydride raw material monomers of polyimide, in particular to a high-yield green and safe synthesis method of 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride. The method comprises the following steps: taking 4-chlorophthalic anhydride as an initial raw material, dissolving the chlorophthalic anhydride in a sodium hydroxide aqueous solution, adding reducing agents or auxiliaries such as cyclodextrin, sorbitol, xylitol, glucose, sucrose, serine and threonine, adding a palladium-carbon catalyst, stirring and reacting for several hours at 90-100 DEG C under the protection of nitrogen, performing filtration, separation and recovery of the palladium-carbon catalyst ((which can be repeatedly used for 8-10 times) while hot, neutralizing filtrate with hydrochloric acid until the pH value is 3-4, generating a large amount of white precipitate, cooling to below 0 DEG C, filtering, washing a filter cake with deionized cold water for multiple times to obtain a 3, 3', 4, 4'-biphenyltetracarboxylic acid product, and dehydrating the product at 200 DEG C to obtain 3, 3', 4, 4'-biphenyltetracarboxylic dianhydride with the yield of more than 90%. The synthesis method is actually a high-yield green and environment-friendly synthesis method of biphenyl tetracarboxylic dianhydride.

Description

technical field [0001] The invention relates to the technical field of synthesis of polyimide acid anhydride raw material monomers, in particular to a high-yield green and safe synthesis method of 3,3',4,4'-biphenyltetracarboxylic dianhydride. Background technique [0002] 3,3',4,4'-Biphenyltetracarboxylic dianhydride (i.e., biphenyltetracarboxylic dianhydride) is the main monomer for the synthesis of high-performance polyimides, especially polyimides for electronic devices. It is co-condensed with 2-(4'-aminophenyl)-5-aminobenzimidazole, 4,4-diaminodiphenyl ether and 1,4'-p-phenylenediamine, and formed by spinning High-temperature, seawater-resistant high-strength and high-modulus polyimide fibers; with 2,2-bis(trifluoromethyl)-4,4-diaminobiphenyl, 2,2-bis(4-aminophenyl)hexafluoropropane, Polyamide formed by cocondensation or copolymerization of 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and 9,9-bis(4-aminophenyl)fluorene and other diamines Imine film has excellen...

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
IPC IPC(8): C07D307/89B01J23/44B01J37/00B01J37/08
CPCC07D307/89B01J23/44B01J37/0009B01J37/0018Y02P20/584
Inventor 侯豪情彭信文赵永丽
Owner JIANGXI NORMAL UNIV
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com