Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of aromatic diether dianhydride

A diether dianhydride and aromatic technology, which is applied in the field of preparation of aromatic diether dianhydride, can solve the problems of difficult purification and increased operation complexity, and achieve the effects of simple process, low production cost and short reaction cycle

Active Publication Date: 2021-02-05
吉林省亚安新材料有限公司
View PDF9 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method shortens the reaction time, but uses a large amount of organic solvent and water, requires multiple extractions and washings, increases the complexity of the operation, and the final diether dianhydride solution is difficult to remove due to the high boiling point solvent , it is more difficult to purify

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 aromatic diether dianhydride
  • Preparation method of aromatic diether dianhydride
  • Preparation method of aromatic diether dianhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation of embodiment 1 bisphenol A type diether dianhydride

[0030] (1) Mix 4-nitrophthalic acid (46.45g, 0.22mol) with xylene (160mL), concentrated sulfuric acid (1.0mL), heat to 50°C, add dropwise tert-butanol (63.1mL, 0.66mol ), monitored by HPLC until the reaction was complete, cooled to 20-30°C after the reaction was complete, added solid sodium hydroxide (2.0g), and stirred for 30 minutes, evaporated xylene (about 140mL) under reduced pressure, added dimethyl ethyl Amide (200mL), standby;

[0031] (2) Mix bisphenol A (22.89g, 0.1mol), sodium hydroxide (8.0g, 0.2mol) and xylene (150mL), reflux under nitrogen atmosphere to remove water to dryness, then distill off xylene (approx. 130mL), cooled to below 100°C to obtain bisphenol disodium salt;

[0032] (3) Add the solution prepared in step (1) to the bisphenol disodium salt prepared in step (2), heat at 140°C for 5 hours, evaporate the solvent (about 200mL) under reduced pressure after the reaction, and ...

Embodiment 2

[0035] The preparation of embodiment 2 bisphenol A type diether dianhydrides

[0036] (1) Mix 4-chlorophthalic acid (44.13g, 0.22mol) with xylene (160mL), concentrated sulfuric acid (1.0mL), heat to 60°C, feed isobutylene gas, and monitor with HPLC until the reaction is complete , cooled to 20-30°C, added solid sodium hydroxide (2.0g), and stirred for 30 minutes, evaporated xylene (about 140mL) under reduced pressure, added dimethylformamide (200mL), set aside;

[0037] (2) Mix bisphenol A (22.89g, 0.1mol), sodium hydroxide (8.0g, 0.2mol) and xylene (150mL), reflux under nitrogen atmosphere to remove water to dryness, then distill off xylene (approx. 130mL), cooled to below 100°C to obtain bisphenol disodium salt;

[0038] (3) Add the solution prepared in step (1) to the bisphenol disodium salt prepared in step (2), heat at 170°C for 5 hours, evaporate the solvent (about 200mL) under reduced pressure after the reaction, and cool down to 60°C Next, add acetic acid (120mL) and...

Embodiment 3

[0041] Embodiment 3 The preparation of 4,4'-triphenylene diether dianhydride

[0042] (1) Mix 4-chlorophthalic acid (44.13g, 0.22mol) with xylene (160mL), p-toluenesulfonic acid (2.0g), heat to 80°C, feed isobutylene gas, and monitor with HPLC until After the reaction is complete, cool to 20-30°C, add solid sodium hydroxide (2.0 g), and stir for 30 minutes, evaporate xylene (about 140 mL) under reduced pressure, add dimethylacetamide (200 mL), and set aside;

[0043] (2) Hydroquinone (11.0g, 0.1mol), sodium hydroxide (8.0g, 0.2mol) and xylene (150mL) were mixed, refluxed to remove water to dryness under a nitrogen atmosphere, and then evaporated xylene ( about 130mL), lower the temperature to below 100°C to obtain bisphenol disodium salt;

[0044] (3) Add the solution prepared in step (1) to the bisphenol disodium salt prepared in step (2), heat at 150°C for 6 hours, evaporate the solvent (about 200mL) under reduced pressure after the reaction, and cool to 60°C Next, add aceti...

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 discloses a preparation method of aromatic diether dianhydride, which comprises the following steps of: by using isobutene or tert-butyl alcohol as a protecting group of carboxyl of chlorinated or nitrophthalic acid, carrying out etherification reaction with disodium bisphenol salt to obtain an intermediate, removing the tert-butyl ester protecting group in the intermediate by usinga small amount of acid without strong alkali treatment to obtain diether tetracarboxylic acid, and finally, enabling the solid tetracarboxylic acid to directly form anhydride at a proper temperature,wherein acetic anhydride dehydration is not needed, and the reaction time of the whole process is only about 21 hours. The preparation method of the aromatic diether dianhydride is short in reaction period, simple and safe in process, high in production efficiency and low in production cost.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and in particular relates to a preparation method of an aromatic diether dianhydride. Background technique [0002] Aromatic diether dianhydride is an important class of chemical raw materials and an important monomer for the preparation of PEI. It can also be used as a curing agent for thermosetting resins and a component of high-temperature-resistant adhesives. The preparation method of traditional aromatic diether dianhydride is to firstly react nitrophthalic anhydride or chlorophthalic anhydride with methylamine or aniline to prepare nitro or chlorophthalimide, and then perform substitution reaction with bisphenol disodium salt to obtain diether Diphthalimide, and then prepare diether dianhydride through strong alkali hydrolysis, acidification and dehydration. The reaction route of these methods is long, and each step needs to be carried out separately, and the next reaction can ...

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): C07D307/89
CPCC07D307/89Y02P20/55
Inventor 李春友
Owner 吉林省亚安新材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com