Method for preparing 4,4'-di(2,4-diamino phenoxy)-3,3',5,5'-tetramethyl diphenyl sulfone

A technology of tetramethyldiphenyl sulfone and diaminophenoxy, which is applied in 4 fields, can solve the problems of no patents and literature reports on the preparation method, and achieve the effects of convenient source of raw materials, less waste, and high yield

Inactive Publication Date: 2008-08-27
DONGHUA UNIV
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 4,4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone is an important aromatic polyvalent primary amine, but its preparation method has not been See patents, literature reports

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 for preparing 4,4'-di(2,4-diamino phenoxy)-3,3',5,5'-tetramethyl diphenyl sulfone
  • Method for preparing 4,4'-di(2,4-diamino phenoxy)-3,3',5,5'-tetramethyl diphenyl sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 63.8 grams (0.1 moles) of 4,4'-bis(2,4-dinitrophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone, 0.7 grams of palladium with a mass percentage of 15 % palladium / charcoal, 1800 milliliters of ethanol and 1800ml ethylene glycol add in the reaction flask, stir, heat up to 60 ℃, start to drip the hydrazine hydrate solution that mass concentration is 60% (hydrazine hydrate molecular weight is 50.06), altogether 250.0 grams ( solution weight). After the dropwise addition of hydrazine hydrate was completed, the stirring reaction was continued for 3.5 hours at a temperature range of 80°C to 90°C, cooled slightly, filtered while hot, cooled mother liquor, added pure water, precipitated crystallized product, filtered, and vacuum-dried to obtain 42.8 grams of 4 , 4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone crystal with a purity of 99.5%, according to the actual obtained 4,4'-bis (2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone amount and theoretical amoun...

Embodiment 2

[0029] 63.8 grams (0.1 mole) of 4,4'-bis(2,4-dinitrophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone, 12.0 grams of palladium mass percentage of 1 % palladium / charcoal, 100ml ethylene glycol and 5800ml ethanol are added in the reaction flask, stirred, heated to 60° C., and the dropwise addition of mass concentration is 85% hydrazine hydrate solution, totally 294.1 grams (solution weight). After the dropwise addition of hydrazine hydrate was completed, the stirring reaction was continued for 5 hours in the temperature range of 80°C to 90°C, cooled slightly, filtered while hot, cooled mother liquor, added pure water, precipitated crystalline product, filtered, and vacuum-dried to obtain 43.3 grams of 4 , 4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone crystal with a purity of 99.2%, according to the actual obtained 4,4'-bis (2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone amount and theoretical amount (51.8 grams), calculated to obtain 4,4'-bis(2,4 The yie...

Embodiment 3

[0031] 63.8 grams (0.1 moles) of 4,4'-bis(2,4-dinitrophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone, 7.8 grams of palladium with a mass percentage of 5 % palladium / charcoal, 600 milliliters of ethanol and 3600ml 2-methoxyethanol are added in the reaction flask, stirred, heated up to 60 ℃, start to drip the hydrazine hydrate solution that mass concentration is 80%, totally 260.0 grams (solution weight) . After the addition of hydrazine hydrate was completed, the stirring reaction was continued at a temperature range of 80°C to 90°C for 5 hours, cooled slightly, filtered while hot, cooling the mother liquor, adding pure water to precipitate a crystalline product, filtering, and vacuum drying to obtain 44.0 g of 4 , 4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone crystal, the purity is 99.7%, according to the actual obtained 4,4'-bis (2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenylsulfone amount and theoretical amount (51.8 grams), calculated to obtain 4,4'-bis(...

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 preparation method of 4, 4'-bis (2, 4-diamino phenoxy)-3, 3', 5, 5'-tetramethyl sulfone, which comprises reacting 4, 4'-bis (2, 4-dinitro phenoxy)-3, 3', 5, 5'-tetramethyl sulfone in a system of palladium / charcoal, hydrazine hydrate solution and saturated fatty alcohol, at 80-90DEG C for 1-5h, filtering immediately, cooling the mother liquor, adding pure water, precipitating white crystal product, filtering and drying in vacuum to obtain 4, 4'-bis (2, 4-diamino phenoxy)-3, 3', 5, 5'-tetramethyl sulfone crystal. The invention has simple operation, eliminatd following refining and extraction, low time consumption, high product yield and high purity (at least 99%), which is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic polyvalent primary amines, in particular to a 4,4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphenyl The preparation method of sulfone. Background technique [0002] Aromatic heterocyclic polymers have excellent thermal stability, nuclear radiation resistance, flame retardancy, organic solvent resistance, and excellent high and low temperature mechanical properties and electrical properties. High-performance fields have been widely used. [0003] With the development of high-performance, lightweight, thin, and refined information electronic products, higher requirements are put forward for the insulating materials of flexible copper clad laminates (FCCL), such as high heat resistance, high strength, and low dielectric constant. and low dielectric loss etc. Therefore, polyimide materials are favored in the field of FCCL. [0004] 4,4'-bis(2,4-diaminophenoxy)-3,3',5,5'-tetramethyldiphe...

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): C07C317/22C07C315/04
Inventor 虞鑫海
Owner DONGHUA UNIV
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