Preparation method of 9,9-bis(4-aminophenyl) fluorene

A technology of diamine fluorene and aniline, which is applied in the field of preparation of bisamine fluorene, can solve the problems of complicated post-processing, low product purity, difficult recovery and the like, and achieves simple post-processing, improved purity and yield, and reduced labor costs. Effect

Inactive Publication Date: 2019-05-10
宏威高新材料有限公司 +2
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing bisamine fluorene, to solve the pr

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 9,9-bis(4-aminophenyl) fluorene
  • Preparation method of 9,9-bis(4-aminophenyl) fluorene
  • Preparation method of 9,9-bis(4-aminophenyl) fluorene

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0039] Example 1

[0040] Step 1: Add 103g of aniline and 11g of hydrochloric acid to a 250ml three-necked flask equipped with a stirrer, thermometer and water separator. After stirring for 10 minutes, add 18g of 9-fluorenone and 50ml of toluene. The temperature will be refluxed for 6-10 hours, and the system will be separated. water;

[0041] Step 2: Cooling, sampling, thin-layer chromatography analysis, after there is no raw material 9-fluorenone, add 13g of 35% NaOH aqueous solution to the system, stir for 30min, heat and reflux, and separate the water in the system;

[0042] Step 3: Recover toluene: increase the temperature, return toluene to the water separator and collect; collect 48ml of toluene, and then extract 77g of aniline from the system under reduced pressure. The recovery rate of toluene and aniline reaches 92%;

[0043] Step 4: Add absolute ethanol to the system to disperse, filter and collect the filter cake, add the filter cake to 150ml of water and stir for 30 minut...

Example Embodiment

[0044] Example 2

[0045] Step 1: Add 515g of aniline and 55g of hydrochloric acid to a 1000ml three-necked flask equipped with a stirrer, a thermometer and a water separator. After stirring for 15 minutes, add 90g of 9-fluorenone and 100ml of toluene. The temperature will be refluxed for 10 hours to separate the water in the system;

[0046] Step 2: Cooling, sampling, thin layer chromatography analysis, after no raw material 9-fluorenone, add 65g of 35% NaOH aqueous solution to the system, stir for 30min, heat up and reflux, and separate the water in the system;

[0047] Step 3: Recover toluene: increase the temperature, return toluene to the water separator and collect; collect 95ml of toluene, and then extract 392g of aniline from the system under reduced pressure. The recovery rate of toluene and aniline is 93%;

[0048] Step 4: Add absolute ethanol to the system for dispersion, filter and collect the filter cake, add the filter cake to 150ml of water and stir for 30 minutes to was...

Example Embodiment

[0049] Example 3

[0050] Step 1: Add 465g of aniline and 75g of hydrochloric acid to a 1000ml three-necked flask equipped with a stirrer, a thermometer and a water separator. After stirring for 15 minutes, add 90g of 9-fluorenone and 100ml of toluene, and reflux for 10 hours to separate the water in the system;

[0051] Step 2: Cooling, sampling, thin-layer chromatography analysis, after there is no raw material 9-fluorenone, add 80g of 40% NaOH aqueous solution to the system, stir for 30min, heat and reflux, and separate the water in the system;

[0052] Step 3: Recover toluene: increase the temperature, return toluene to the water separator and collect; collect 95ml of toluene, and then extract 353g of aniline from the system under reduced pressure. The recovery rate of toluene and aniline is 95%;

[0053] Step 4: Add absolute ethanol to the system for dispersion, filter and collect the filter cake, add the filter cake to 150 ml of water and stir for 30 minutes to wash off the salt ...

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 provides a preparation method of 9,9-bis(4-aminophenyl) fluorine and relates to the technical field of fine chemical engineering. The 9,9-bis(4-aminophenyl) fluorine is prepared by using9-fluorenone and aniline as the raw materials and hydrochloric acid as the catalyst. The preparation method has the advantages that aniline hydrochloride is replaced by the hydrochloric acid to serveas the catalyst of 9,9-bis(4-aminophenyl) fluorine synthesizing, and reaction cost is lowered; the recovery rate of the aniline and toluene reaches up to 92-95% by using one-pot post-processing and purification, the recovered aniline and toluene can be used repeatedly, and environment protection is achieved; the post-processing is simple, waste liquid is reduced, labor cost is lowered, the yieldof the product 9,9-bis(4-aminophenyl) fluorine can reach 89% or above, and product purity and yield are increased effectively.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of bisamine fluorene. Background technique [0002] Bisamine fluorene, whose scientific name is 9,9-bis(4-aminophenyl)fluorene [9,9-bis(4-aminophenyl)fluorene, BPF], is an important chemical intermediate. It is mainly used in the synthesis of high thermal stability aromatic polyimide and epoxy resin. Bisamine fluorene derivatives are also excellent hole-transporting materials in organic and polymer light-emitting semiconductors, with good blue light characteristics, high glass transition temperature and high thermal stability. Diamine fluorene can also be used in fuel cells, which can improve the electrical conductivity, mechanical stability, thermal stability and chemical stability of the battery. In addition, bisamine fluorene can also be used in liquid crystal display alignment materials and polarizing polymer materials. In recent years, the rese...

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): C07C213/00C07C213/08C07C215/70C07C209/68C07C211/45C07C211/50
Inventor 不公告发明人
Owner 宏威高新材料有限公司
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