3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salts and preparation method thereof

A technology of alkylphosphinyl propyl phenyl and alkyl phosphinyl propyl ether, which is applied in the field of organic phosphinous compounds and their preparation, can solve problems such as hindering industrial development and lagging behind, and achieve the goal of not producing three wastes pollution, Good thermal stability, easy charring and anti-dripping effect

Active Publication Date: 2014-12-10
SUZHOU UNIV OF SCI & TECH
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the development of organic phosphine flame retardants in China is relatively lagging behind, and there is a strong demand for organic phosphine flame retardants with excellent cost performance in the market, which seriously hinders the development of related industries
And because there are many kinds of polymer materials and there are many kinds of flame retardants that are required to be compatible, there is an urgent need for the development of new organic phosphine flame retardants.

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
  • 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salts and preparation method thereof
  • 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salts and preparation method thereof
  • 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salts and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Self-made anhydrous hypophosphorous acid-acetic acid solution, add 25.4g (0.24mol) sodium hypophosphite monohydrate and 100ml acetic acid into a 500ml three-neck flask, stir and dissolve, add 12g concentrated sulfuric acid dropwise, stir for 0.5h, cool and filter Remove sodium sulfate hydrate, wash the filter cake with 100ml acetic acid, and take the filtrate to obtain anhydrous hypophosphorous acid-acetic acid solution.

[0032] The resulting anhydrous hypophosphorous acid-acetic acid solution was added to a 500ml three-necked flask, heated to 90°C, and then 20.9g (0.12mol) of allylphenyl allyl ether and 1.16g of benzoyl peroxide were dissolved. Dissolve it in 100ml of acetic acid, and slowly add it to a three-necked flask within 6 hours. After the addition, keep it warm for 2 hours, cool it down, pour all the reaction solution into a 500ml high-pressure reactor, exhaust the air in the reactor, and heat up to 90°C, start to feed ethylene, set the pressure of ...

Embodiment 2

[0033] Example 2 Self-made anhydrous hypophosphorous acid-acetic acid solution, the operation method is the same as that in Example 1. Add 0.24mol of self-made anhydrous hypophosphorous acid-acetic acid solution into a 500ml three-necked flask, heat up to 110°C, and then dissolve 20.9g (0.12mol) allyl phenyl allyl ether and 0.94g tert-butyl peroxybenzoate are dissolved in 100ml acetic acid, and it is slowly added in the there-necked flask in 6h, after adding, keep warm for 2h, cool, and All the reaction solution is poured into a 500ml high-pressure reactor, the air in the reactor is exhausted, the temperature is raised to 110° C., and ethylene is started to be introduced. The acetic acid solution of tert-butyl oxide is poured into the reaction kettle with a constant flow pump, and the temperature is controlled not to exceed 115°C. When the ethylene consumption no longer increases, the constant flow pump is turned off, and the reaction is carried out at constant temperature and ...

Embodiment 3

[0034] Example 3 Self-made anhydrous hypophosphorous acid-acetic acid solution, the operation method is the same as that in Example 1. Add 0.18mol of self-made anhydrous hypophosphorous acid-acetic acid solution into a 500ml three-necked flask, heat up to 90°C, and then dissolve 20.9g (0.12mol) allyl phenyl allyl ether and 0.6 g of azobisisobutyronitrile were dissolved in 100 ml of acetic acid, and slowly added to the three-necked flask within 6 hours. Pour it into a 500ml high-pressure reactor, exhaust the air in the reactor, heat up to 90°C, start feeding ethylene, set the pressure of the ethylene pressure reducing valve to 0.6MPa, and simultaneously inject 0.6g of azobisisobutyronitrile The acetic acid solution was poured into the reaction kettle with a constant flow pump, and the temperature was controlled not to exceed 95°C. When the ethylene consumption no longer increased, the constant flow pump was turned off, and the reaction was carried out at constant temperature and...

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 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salts and a preparation method thereof. The compounds have a structure shown as the specification. In the structural formula, R refers to ethyl or propyl; and M refers to Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Ce, Fe, Mn, Li, Na or K metal ion, and q is the valence of M. The preparation method comprises the following steps: reacting phosphinic acid or alkali metal salt of phosphinic acid with allyl propyl allyl ether and olefin in the presence of a radical initiator to obtain 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether or alkali metal salts of 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether; and reacting with a metal compound to obtain a corresponding 3-alkyl phosphinic propyl phenyl-3-alkyl phosphinic propyl ether metal salt. The compounds are stable in performance, nontoxic, and high in flame retardancy, has good compatibility with high polymer materials, and can serve as flame retardants for polyester, polyamide, epoxy resins, fiberglass resins, coatings and the like; and the process is simple and suitable for large-scale production.

Description

technical field [0001] The invention relates to an organic phosphine compound and a preparation method thereof, in particular to a 3-alkylphosphinopropyl phenyl-3-alkylphosphinopropyl ether metal salt and a preparation method thereof. The compound can be Used as a flame retardant for polyester, polyamide, epoxy resin, fiberglass resin, coating, etc. Background technique [0002] At present, due to the advantages of low smoke, low toxicity and no pollution, halogen-free organic phosphine flame retardants are favored by people. The development of environmentally friendly organic phosphine flame retardants has become a research hotspot in the field of flame retardant technology. However, the development of organic phosphine flame retardants in China is relatively lagging behind, and there is a strong demand for organic phosphine flame retardants with excellent cost performance in the market, which seriously hinders the development of related industries. And because there are m...

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): C07F9/30C08K5/5313C08L67/02
Inventor 王彦林杨兴
Owner SUZHOU UNIV OF SCI & 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