Preparation method of 3,3',4,4'-tetra carboxylic acid biphenyl

A technology of biphenyltetracarboxylic acid and phthalic acid, applied in 4 fields, can solve the problems of low yield, poor production efficiency and economic benefit, and high cost, and achieves high yield, high production efficiency and economic benefit, and low cost Effect

Active Publication Date: 2009-12-23
HEBEI HAILI FRAGRANCES CO LTD
View PDF1 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned methods all have the disadvantages of low yie

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
  • Preparation method of 3,3',4,4'-tetra carboxylic acid biphenyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 18g (0.45mol) of sodium hydroxide and 200ml of water to a four-necked reaction flask equipped with a dropping funnel, a thermometer, and stirring, heat up to 80°C, and after dissolving and transparent, add 15g (0.075mol) of 4-chloro-o- Phthalic acid, add 0.3g of the above-mentioned carbon catalyst, heat up to 90°C, add 3g of methanol dropwise, and the dropwise addition time is 4 hours. After the dropwise addition, keep the temperature for 3 hours, filter, and add the mother liquor dropwise to 10% sulfuric acid solution to obtain White crystals were filtered while hot and washed with water to obtain crude biphenyl tetracarboxylic acid.

[0026] Put the crude biphenyltetracarboxylic acid in 10 times purified water, boil it in water at 100°C for 5 hours, cool down, wash with water, and dry to obtain 10.1 g of biphenyltetracarboxylic acid with a measured yield of 82%, a purity of 99.7%, and a melting point of 298-300°C.

Embodiment 2

[0028] Add 14g (0.25mol) of potassium hydroxide and 250ml of water to a four-necked reaction flask equipped with a dropping funnel, a thermometer and stirring, and raise the temperature to 80°C. After dissolving and becoming transparent, add 12.3g of 4-bromophthalic acid in portions (0.05mol), add 0.1g of the above-mentioned catalyst, heat up to 95°C, add 5g glycerin aqueous solution dropwise, and the dropwise addition time is 2-5 hours. , white crystals were obtained, filtered while hot, and washed with water to obtain crude biphenyltetracarboxylic acid.

[0029] The crude biphenyltetracarboxylic acid was placed in 8 times purified water, boiled at 100°C for 4 hours, filtered, washed with water, and dried to obtain 7.4g of biphenyltetracarboxylic acid with a measured yield of 89.7%, a purity of 99.6%, and a melting point of 297-299°C.

Embodiment 3

[0031] Add 14g (0.25mol) of potassium hydroxide and 220ml of water to a four-necked reaction flask equipped with a dropping funnel, a thermometer and stirring, raise the temperature to 80°C, and after it dissolves transparently, add 11.7g of 4-iodophthalic acid in portions (0.04mol), add 0.1g of the above catalyst, raise the temperature to 95°C, add dropwise 1g of methanol solution, the dropwise addition time is 2-5 hours, after the dropwise addition, keep warm for 5 hours, filter, and add the mother liquor dropwise to 10% sulfuric acid solution , white crystals were obtained, filtered while hot, and washed with water to obtain crude biphenyltetracarboxylic acid.

[0032] The crude biphenyltetracarboxylic acid was placed in 8 times purified water, boiled at 100°C for 3 hours, filtered, washed with water, and dried to obtain 5.95g of biphenyltetracarboxylic acid with a measured yield of 90%, a purity of 99.5%, and a melting point of 297-299°C.

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

PropertyMeasurementUnit
Melting pointaaaaaaaaaa
Melting pointaaaaaaaaaa
Login to view more

Abstract

The invention provides a preparation method of 3,3',4,4'-tetra carboxylic acid biphenyl and relates to the technical field of organic material preparation. The method mainly comprises the following steps: preparing 3-10% of alkali solution, adding 4-halogenated phthalic acid in the alkali solution, dissolving; adding palladium carbon-potassium iodide binary compound catalyst, dripping alcohols at 80-100 DEG C for 3-8h, after completing the reaction filtrating the solution to obtain the palladium carbon-potassium iodide catalyst; adding the filtrate in 5-10% of sulfuric acid, filtrating the solution to obtain raw tetra carboxylic acid biphenyl and finally refining the raw product; wherein, the molar ratio of COOH in 4-halogenated phthalic acid to OH- in the alkali solution is 1 to 2-3 and the molar ratio of the additive functional hydroxyl of alcohols to 4-halogenated phthalic acid is 1 to 1-3. The invention overcomes the defects of the prior art, and has the outstanding advantages of unique method, simple process, easy operation, high yield, low cost, high production efficiency and economic benefit and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical organic materials, and in particular relates to a preparation method of 4,4'-biphenyltetracarboxylic acid. Background technique [0002] 3,3',4,4'-biphenyltetracarboxylic acid (BPTA) is dehydrated to obtain 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), which is an important polymer - polyimide The precursor can be polymerized with polyfunctional amines to form polyimide. Polyimide is the super heat-resistant resin with the highest heat-resistant temperature so far, and has excellent hydrolysis resistance, mechanical properties and flexibility. It can be used to make Heat-resistant photosensitive resins, optical filters, liquid crystal displays, cross-linked adhesives for conductors and semiconductors, and can also be used in lasers, lithium batteries, and protective materials used in space. [0003] There are a lot of literature reports about BPTA synthesis, such as t...

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): C07C63/331C07C51/353B01J27/08B01J23/44B01J37/00
Inventor 李文革胡国田张云堂杨中民
Owner HEBEI HAILI FRAGRANCES CO LTD
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