Single molecular expansion type alkyl phosphinate flame retardant and preparation method thereof

A technology of alkyl phosphinate and methyl propionate phosphinic acid is applied in the field of flame retardant materials, which can solve the problems of great influence on physical and mechanical properties of substrates, easy deliquescence and precipitation, and low thermal stability, etc. Achieve the effect of retaining mechanical properties, good anti-migration, and preventing migration

Active Publication Date: 2017-07-21
HONGHU YITAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Intumescent flame retardants include two types of multi-component intumescent flame retardants and single-component intumescent flame retardants, among which multi-component intumescent flame retardants such as ammonium polyphosphate (APP), pentaerythritol (PER), melamine The intumescent flame retardant compounded in a certain proportion, the thermal stability of the acid source, carbon source, and gas source is not high, and it is easy to deliquesce and precipitate during application, and the addition amount is large. The physical and mechanical properties of the base material are greatly affected, and the application is limited; therefore, it is necessary to design a one-component intumescent flame retardant with good compatibility with polymers and high thermal stability, and integrate the "three sources" On a macromolecule, a group similar to the structure of the polymer improves the compatibility with the polymer, and introduces an alkyl phosphinate structure to improve thermal stability

Method used

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  • Single molecular expansion type alkyl phosphinate flame retardant and preparation method thereof
  • Single molecular expansion type alkyl phosphinate flame retardant and preparation method thereof
  • Single molecular expansion type alkyl phosphinate flame retardant and preparation method thereof

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preparation example Construction

[0029] The preparation method of unimolecular expansion type alkyl phosphinate flame retardant of the present invention comprises the following steps:

[0030] 1) Hydrolysis acid production: 2-methyl-2,5-dioxo-1,2-oxophospholane is hydrolyzed to obtain methylpropionyl phosphinic acid; the solvent used in the hydrolysis reaction is water or acetone, Or a mixture of water and acetone; the temperature of the hydrolysis reaction is 40-100°C, and the reaction time is 0.5-3h;

[0031]2) Esterification reaction or esterification reaction and amidation reaction: carry out esterification reaction or esterification reaction and amidation reaction with methyl propionyl phosphinic acid and nitrogen-containing polyhydroxy compound to obtain nitrogen-containing ester-containing alkyl Phosphinic acid; wherein the nitrogen-containing polyhydroxy compound is one of the compounds having at least two hydroxyl groups, wherein the nitrogen-containing moiety can be amino or other nitrogen-containin...

Embodiment 1

[0036] Dissolve 1 mol of 2-methyl-2,5-dioxo-1,2-oxaphospholane in 5 mol of acetone at 50°C, slowly add 1 mol of water, stir and reflux for about 1 hour, filter and dry to obtain Methyl propionyl phosphinic acid; 3 mol of the above methyl propionyl phosphinic acid and 1 mol of 1,3,5-tris (2-hydroxyethyl) isocyanurate were added to a container containing 3 times the volume In a toluene flask, stir and reflux at 140°C for 4 hours, cool, pour off the upper layer solution to obtain colorless and transparent 1,3,5-tris(2-hydroxyethyl)isocyanurate methylpropionic acid Triester phosphinic acid; at normal temperature, add 1 times the volume of distilled water to the above 1mol nitrogen-containing ester-containing alkylphosphinic acid, stir until it dissolves into a homogeneous solution, then add NaOH aqueous solution dropwise to adjust the volume of the solution When the pH value reaches 7.0, 1,3,5-tris(2-hydroxyethyl)isocyanurate methyl propionate triester sodium phosphinate aqueous s...

Embodiment 2

[0049] Dissolve 1 mol of 2-methyl-2,5-dioxo-1,2-oxaphospholane in 5 mol of acetone at 40°C, slowly add 1 mol of water, stir and reflux for about 0.5 hours, filter and dry to obtain Methyl propionyl phosphinic acid; 3 mol of the above methyl propionyl phosphinic acid and 1 mol of 1,3,5-tris (2-hydroxyethyl) isocyanurate were added to a container containing 3 times the volume In a xylene flask, stir and reflux at 160°C for 2 hours, cool, pour off the upper solution to obtain colorless and transparent 1,3,5-tris(2-hydroxyethyl)isocyanurate methylpropane Acid triester phosphinic acid; at room temperature, add 1 times the volume of distilled water to the above 1 mol of nitrogen-containing ester-containing alkyl phosphinic acid, stir until it dissolves into a homogeneous solution, and then add NaOH aqueous solution dropwise to adjust the solution pH value to 7.0, to obtain 1,3,5-three (2-hydroxyethyl) isocyanurate methyl propionate triester sodium phosphinate aqueous solution; The ...

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Abstract

The invention discloses a single molecular expansion type alkyl phosphinate flame retardant. A structural general formula is shown in the description, a molecular structure is starlike, R-O- is a hydroxyl dehydrogenized structure after a nitrogen-containing polyhydroxy compound is subjected to esterification reaction, the formula (shown in the description) is a hydroxyl removed structure provided with molecular hydroxyl and obtained after organic phosphonic acid esterification reaction, n corresponds to the number of hydroxy and amidogen of the nitrogen-containing polyhydroxy compound, and M is a metal or semi-metal having the valence m. The invention further discloses a preparation method the flame retardant. The three-source proportion of the flame retardant can be regulated and controlled by selecting different nitrogen-containing polyhydroxy compounds. The molecular structure contains P-C keys and has excellent heat stability and good chemical properties. A specific carboxylic ester structure has good mixing compatibility with a polymer, and the original mechanical properties of the polymer can be retained to the greater degree. Metal ions in molecules can prevent the flame retardant from migrating from the polymer and meanwhile have a catalytic charing effect.

Description

technical field [0001] The invention relates to a novel flame retardant, which belongs to the technical field of flame retardant materials, in particular to a monomolecular expansion type alkyl phosphinate flame retardant and a preparation method thereof. Background technique [0002] Phosphorus-based flame retardants have become the main direction of the development of environmentally friendly flame retardants because the charcoal layer formed by them has good heat insulation, oxygen insulation, smoke suppression and anti-melt droplet effects, and phosphorus-based flame retardants are the main ones. The component intumescent flame retardant (IFR) is a multi-element synergistic composite flame retardant. Intumescent flame retardants include two types of multi-component intumescent flame retardants and single-component intumescent flame retardants, among which multi-component intumescent flame retardants such as ammonium polyphosphate (APP), pentaerythritol (PER), melamine T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C07F9/6521C08K5/5313C08L67/00
CPCC07F9/301C07F9/6521C08K5/5313C08L2201/02C08L67/00
Inventor 邹立勇刘继延刘学清陈佳周敏
Owner HONGHU YITAI TECH CO LTD
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