Preparation method of high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative

A derivative and high-purity technology, applied in the field of flame retardants, can solve problems affecting applications and achieve short reaction routes

Active Publication Date: 2013-11-27
JIANGSU YOKE TECH
View PDF2 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent uses DOPO and ethylene glycol (EG) as raw materials to synthesize the DOPO derivatives, and the resulting product is a mixture of three isomers (enantiomers) of compound I, of which compound I (RS type) The melting point is the highest, due to the existence of two other low-melting point isomers (RR

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 high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative
  • Preparation method of high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative
  • Preparation method of high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0017] Example 1. Preparation of DOPO derivative compound I (with catalyst I)

[0018] Add CDOP (47 g, 0.20 mol), triethylamine (20.24 g, 0.20 mol), sodium iodide (1.50 g) and 100ml xylene into the flask. While stirring, slowly add ethylene glycol (4.97 g , 0.08 mol), keep the system temperature no more than 20 degrees during the dripping process. After the addition, react at 20 degrees for 2 hours, and then heat up to 120 degrees for 3 hours. After cooling, filter, add 100 mL of ethanol to the filtrate, stir for half an hour at 80 degrees, and filter while hot to obtain 30.4 g of product with a yield of 83%. (Because the excess CDOP can be recycled, the yield is calculated based on ethylene glycol).

Example Embodiment

[0019] Example 2. Preparation of DOPO derivative compound I (without catalyst I)

[0020] Add CDOP (70.4 g, 0.30 mol), iodine (2.0 g) and 80ml of diphenylmethane to the flask, heat to 160 degrees, and then slowly add ethylene glycol (9.31 g, 0.15 mol) to the flask. The reaction was continued for 20 hours at temperature. Cool to about 80 degrees, add 90 mL of ethanol to the system, stir for half an hour, and filter while hot to obtain 55.1 g of product with a yield of 80%.

Example Embodiment

[0021] Examples 3-19, referring to Examples 1 and 2, modify some parameters, as shown in the following table:

[0022]

[0023] In this table, as in Example 3, the reaction temperature is 10 / 120 and the reaction time is 3 / 12, which means that the temperature of the system should not exceed 10 degrees during the dripping of ethylene glycol, and the reaction will be at about 10 degrees for 3 hours after the addition. , And then heat up to 120 degrees for 12 hours, the same applies to other examples.

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 a high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative, and relates to a flame retardant in the field of chemical materials. According to the preparation method, CDOP (10-chloro-9,10-dihydro-9-oxa-10-phosphaphenanthrene) is used as a raw material and reacts with ethylene glycol under the action of a catalyst, wherein the reaction temperature is 10-200 DEG C, and the reaction time is 5 to 30 hours, so that a product with high optical purity can be directly obtained. The preparation method has the advantages that reaction routes are short, the product does not contain another two isomers, and the melting point of the product reaches up to about 300 DEG C. The high-purity DOPO derivative can be used as the flame retardant.

Description

technical field [0001] The invention relates to a flame retardant in the field of chemical materials, in particular to a preparation method of a high-purity DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) derivative. Background technique [0002] Epoxy resins are widely used in various electronic components, electrical equipment, automotive parts, and sports facilities due to their special properties such as adhesion, heat resistance, and moldability. At present, brominated flame retardants account for a large proportion of epoxy resins related to the electrical and electronic fields, such as copper clad laminates and printed circuit boards. However, based on the consideration that halogens can cause harm to the environment and human safety, the more environmentally friendly phosphorus-based flame retardants have gradually received attention. In the field of epoxy resin sheets, the application of additive phosphorus flame retardants is relatively rare, because it ...

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): C07F9/6574
Inventor 沈琦陈杜刚吴俊东刘明霞
Owner JIANGSU YOKE TECH
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