Unlock instant, AI-driven research and patent intelligence for your innovation.

A polymeric phosphorus-silicon flame retardant containing dopo side groups and preparation method thereof

A DOPO-AA, DOPO-CH2OH technology, used in the field of flame retardants, can solve the problems of affecting applicability, the unadjustable ratio of phosphorus and silicon elements, etc., and achieve good carbon formation, improved limiting oxygen index, and good thermal stability. Effect

Inactive Publication Date: 2016-01-06
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yang Shiyong's research group has applied for patents on a variety of phosphorus-silicon synergistic flame retardants. These compounds have the characteristics of hydrolysis resistance, easy purification and good synergistic effect, thus endowing common polymer materials with excellent flame retardant properties (CN201210479147.4; CN201210063638.0; ZL200710178086.7); However, the ratio of phosphorus and silicon elements in the flame retardants involved in these patents cannot be adjusted, which affects its applicability in different materials

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
  • A polymeric phosphorus-silicon flame retardant containing dopo side groups and preparation method thereof
  • A polymeric phosphorus-silicon flame retardant containing dopo side groups and preparation method thereof
  • A polymeric phosphorus-silicon flame retardant containing dopo side groups and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add DOPO-CH to a three-neck round bottom flask with temperature, magnetic stirrer, condenser, and addition 2 OH, 49.2g (0.2mol), 22.3g (0.22mol) triethylamine, 200ml chloroform, the reaction solution was cooled to -20°C under stirring, and 20.0g (0.22mol) propylene was added dropwise in about 1.5 hours at this temperature 50ml of chloroform solution of acid chloride, after the dropwise addition, continue to react at about -10°C for 4 hours, and react at 20°C for 4 hours; The crude product was obtained after removal of chloroform. The product uses ethyl acetate as the mobile phase, and is purified by neutral silica gel column chromatography. After removing the ethyl acetate, it is frozen to accelerate crystallization to obtain a yellow solid product. figure 1 Proton NMR spectrum (CD) of DOPO-AA 3 Cl); figure 2 NMR phosphorous spectrum (CD) of DOPO-AA 3 Cl).

Embodiment 2

[0026] Add 80g (0.28mol) of DOPO-AA and 30g (0.12mol) of KH570 into the reactor, dissolve with DMF, add 0.55g of BPO, react in an oil bath at 80°C for 10 hours, pour the reaction product into ethanol for washing Suction filtration, the solid obtained after drying is the copolymerization product [Poly(DOPO-AA-co-KH570)73], and its thermal weight loss curve in air is shown in the attached image 3 .

Embodiment 3

[0028] Add 69g (0.24mol) of DOPO-AA and 40g (0.16mol) of KH570 into the reactor, dissolve with DMF, add 0.55g of BPO, react in an oil bath at 80°C for 10 hours, pour the reaction product into ethanol for washing Suction filtration, the solid obtained after drying is the copolymerization product [Poly(DOPO-AA-co-KH570)64], and its thermal weight loss curve in air is shown in the attached image 3 .

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

PropertyMeasurementUnit
oxygen indexaaaaaaaaaa
Login to View More

Abstract

A polymeric phosphorus-silicon flame retardant containing DOPO side groups disclosed in the present invention has a repeating unit structure as shown in formula I. The present invention adjusts the ratio of comonomers through free radical copolymerization, and prepares a polymeric flame retardant with adjustable phosphorus and silicon ratios. The flame retardant has the characteristics of good thermal stability, good char formation, and migration resistance; the phosphorus and silicon elements in the molecular structure can play a synergistic role, thus endowing polystyrene with excellent flame retardancy; it is expected to be applied to other Common polymer materials.

Description

technical field [0001] The invention belongs to the field of flame retardants, and relates to a structure of a polymeric phosphorus-silicon flame retardant containing DOPO side groups and a preparation method thereof. Background technique [0002] In recent years, with the continuous improvement of awareness of environmental protection and safety protection, the development of halogen-free flame retardants has become a key technology in the field of flame retardants. Around 9,10-dihydro-9-oxa-10-phosphaphenanthrene Oxides (abbreviated as DOPO) and their derivatives are mostly small molecular compounds, which have the disadvantages of poor compatibility, poor thermal stability, and poor droplet resistance (for example, CN1910263A). Polymeric flame retardants can significantly improve the deficiencies of small molecule flame retardants. CN200910144202.2 discloses a polymeric phosphorus-containing flame retardant (I) whose side group is DOPO, which is used for flame retardant ...

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 Patents(China)
IPC IPC(8): C08F230/02C08F230/08C08L43/02C08L25/06
Inventor 闫莉尚宏周桑晓明李婷婷张志明
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY