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

Method for preparing hexa(4-carboxylphenoxy)cyclotriphosphazene by hydrogen peroxide oxidation

A technology of cyclotriphosphazene and phenoxy, which is applied in the field of preparation of hexa-cyclotriphosphazene, can solve the problems of cumbersome post-processing, and achieve the effects of simple post-processing operation, accelerated reaction rate, and lower reaction temperature

Inactive Publication Date: 2013-12-25
BEIJING INSTITUTE OF TECHNOLOGYGY +1
View PDF4 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The post-processing of this method is more cumbersome

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 hexa(4-carboxylphenoxy)cyclotriphosphazene by hydrogen peroxide oxidation
  • Method for preparing hexa(4-carboxylphenoxy)cyclotriphosphazene by hydrogen peroxide oxidation
  • Method for preparing hexa(4-carboxylphenoxy)cyclotriphosphazene by hydrogen peroxide oxidation

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] A kind of preparation method of hexa(4-carboxy-phenoxy)-cyclotriphosphazene of the present invention, adopts two-step method in essence, comprises the preparation of HAPCP and the oxidation reaction two steps of HAPCP:

[0025] (1) Preparation of intermediate product HAPCP

[0026] A. Weigh the raw materials 4-hydroxybenzaldehyde, acid-binding agent and HCCP, wherein the molar (substance amount) ratio of 4-hydroxybenzaldehyde, acid-binding agent and HCCP is 5-10:5-8:1.

[0027] B. Add an acid-binding agent (anhydrous potassium carbonate or anhydrous potassium phosphate) into the reaction vessel, then dissolve 4-hydroxybenzaldehyde in anhydrous THF, add it dropwise to the reaction vessel, stir for 0.2-2h, and The temperature of the system rises to 50-80°C, dissolve HCCP in anhydrous THF, add the anhydrous THF solution of HCCP into the constant pressure dropping funnel, add dropwise to the above reaction system at an appropriate speed, and heat and stir , After the dropw...

Embodiment 1

[0037] In a 250ml dry three-necked flask equipped with a magnet, a thermometer, a constant pressure dropping funnel, and a condensing reflux device, add crushed and dried k 2 CO 3 9.67g of powder, then dissolve 9.76g of 4-hydroxybenzaldehyde in 80ml of anhydrous THF, add it dropwise into a three-necked flask, react for 40min under stirring conditions, raise the temperature of the system to 67°C, and dissolve 3.48g of HCCP in 30ml of anhydrous THF In THF water, after the solid was completely dissolved, it was added dropwise to the reaction system for about 1 hour, and the system was refluxed at 70°C for 24 hours.

[0038] After the reaction, a white turbid solution was obtained, and the solid KCl and K were removed by suction filtration. 2 CO 3 Etc. Concentrate the filtrate to about 50ml with a rotary evaporator, pour the concentrated solution into 200ml deionized water, a white precipitate appears immediately, filter, and wash the product 3 times with deionized water repeate...

Embodiment 2

[0041] In a 500ml dry three-necked flask equipped with a magnet, a thermometer, a constant pressure dropping funnel and a condensing reflux device, add crushed and dried k 2 CO 3 16.58g of powder, then dissolve 17.08g of 4-hydroxybenzaldehyde in 130ml of anhydrous THF, add it dropwise into a three-necked flask, react for 30min under stirring conditions, raise the temperature of the system to 50°C, and dissolve 6.95g of HCCP in 50ml of anhydrous THF In THF water, after the solid was completely dissolved, it was added dropwise to the reaction system for about 1.5 hours, and the system was refluxed at 67°C for 30 hours.

[0042] After the reaction, a white turbid solution was obtained, and the solid KCl and K were removed by suction filtration. 2 CO 3 Etc. Concentrate the filtrate to about 40ml with a rotary evaporator, pour the concentrated solution into 300ml deionized water, a white precipitate appears immediately, filter, and wash the product 3 times with deionized water re...

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 method for preparing hexa(4-carboxylphenoxy)cyclotriphosphazene by hydrogen peroxide oxidation. The method comprises: taking hexachlorocyclotriphosphazene (HCCP) and 4-hydroxybenzaldehyde as raw materials and taking anhydrous tetrahydrofuran as a solvent, adding an acid binding agent, performing a nucleophilic substitution reaction to prepare hexa(4-formacylphenoxy) cyclotriphosphazene (HAPCP); and performing filtering, underpressure distillation and recrystallization purification, then under an alkaline condition, oxidizing hexa(4-formacylphenoxy) cyclotriphosphazene with hydrogen peroxide to obtain hexa(4-carboxylphenoxy)cyclotriphosphazene (HCPCP). The molar ratio of 4-hydroxybenzaldehyde, the acid binding agent and HCCP is (5-10):(5-8):1, the temperature of the nucleophilic substitution reaction is 50-80 DEG C and the reaction time is 10-30 h. Compared with the prior art, the method of the invention has the advantages of mild reaction condition, more thorough reaction, reduced reaction temperature, accelerated reaction speed and improved product yield and purity.

Description

technical field [0001] The present invention relates to a kind of preparation method of hexa(4-carboxy-phenoxy)-cyclotriphosphazene, in particular to a method for preparing hexa(4-carboxy-phenoxy)-cyclotriphosphazene by hydrogen peroxide oxidation method. Background technique [0002] Since HCCP was identified as a ring structure in phosphazene compounds at the end of the 19th century, phosphazene compounds have been developed rapidly. Phosphazenes are divided into two types: cyclic phosphazenes and linear phosphazenes. Cyclic phosphazenes are not only important intermediates for the synthesis of linear phosphazenes, but are also favored for their combination of stability and activity. Since the 1980s, foreign countries have begun to study cyclophosphazene derivatives, which have developed rapidly due to the proposal of halogen-free flame retardants in recent years. Professor Allcock of the University of Pennsylvania synthesized HAPCP in 1981 and performed a series of cha...

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): C07F9/6593C08K5/5399C08L63/00
Inventor 刘吉平宝冬梅宋仁学宋仁江卢正中
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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