Single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant as well as preparation method and application thereof

A technology of intumescent flame retardants and macromolecules, which is applied in the field of one-component phosphorus-nitrogen bicyclic cage macromolecular intumescent flame retardants and its preparation, and can solve the problems of poor compatibility and easy migration of polymer matrix , to achieve good compatibility, overcome easy migration, and save costs

Active Publication Date: 2016-05-04
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to address the shortcomings of existing intumescent flame retardants, and provide a single-component phosphorus-nitrogen bicyclic cage macromolecular intumescent flame retardant, which can effectively overcome the small molecule intumescent flame retardants. Eliminates the disadvantages of easy migration of agents, easy moisture absorption, and poor compatibility with the polymer matrix, and endows the polymer with good flame retardancy and water resistance

Method used

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  • Single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant as well as preparation method and application thereof
  • Single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant as well as preparation method and application thereof
  • Single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Synthesis of 1-oxo-4-hydroxymethyl-1-phospha-2,6,7-trioxabicyclo[2.2.2]octane (PEPA): add 150mL di Hexane and 34.04g (0.25mol) of pentaerythritol, heated to 95 ° C, mechanically stirred for 30min; 38.33g (0.25mol) of phosphorus oxychloride dissolved in 50mL of dioxane, dropwise added to the flask within 1h, and Dissolve 30.00g (0.75mol) of sodium hydroxide in 120mL of deionized water to prepare an acid-binding agent, and add it dropwise to the flask at the same time, and continue to react for 4 hours after the drop is completed; after the reaction is completed, let it stand for cooling, concentrate and filter the mixture, Wash with dioxane and ethanol successively, and then dry to obtain white solid powder PEPA.

[0036]2) Synthesis of one-component phosphorus-nitrogen bicyclic cage macromolecular expansion flame retardant (PECA): Add 200mL dioxane, 18.44g (0.1mol ) cyanuric chloride and 18.01g (0.1mol) PEPA, mechanically stirred for 30min, 4g (0.1mol) sodium hydrox...

Embodiment 2

[0041] The difference between this example and Example 1 is that the reaction temperature in the 50°C reaction stage in step 2) is increased to 55°C, and 3.01g (0.05mol) of 1,2-ethylenediamine is replaced by 5.41g (0.05mol) For 1,4-phenylenediamine, the dropping time is extended to 2.5 hours, and the reaction time is extended to 4 hours after the dropping; the reaction temperature in the 95°C reaction stage is raised to 100°C, and 3.01g (0.05mol) of 1,2-ethylenediamine is replaced 5.41g (0.05mol) of 1,4-phenylenediamine was obtained, the amount of sodium hydroxide was increased to 4.4g (0.11mol), the dropping time was extended to 2.5h, and the reaction time was extended to 6h after the dropping. The obtained product is a white solid powder, and its structural formula is shown in the following formula. The benzene ring introduced by phenylenediamine is also an important carbon source, and has good thermal stability, and the resulting carbon layer has a stable structure. The av...

Embodiment 3

[0044] The difference between this example and Example 1 is that the reaction temperature in the 50°C reaction stage in step 2) is raised to 60°C, and 3.01g (0.05mol) of 1,2-ethylenediamine is replaced by 9.91g (0.05mol) For 4,4'-diaminodiphenylmethane, the dropwise addition time was extended to 3h, and the reaction time was extended to 5h after the dropwise completion; the reaction temperature was raised to 105°C in the 95°C reaction stage, and 3.01g (0.05mol) of 1,2-ethanedi The amine was replaced by 9.91g (0.05mol) of 4,4'-diaminodiphenylmethane, the amount of sodium hydroxide was increased to 4.4g (0.11mol), the dropping time was extended to 3h, and the reaction time was extended to 7h after the dropping. The obtained product is a white solid powder, and its structural formula is shown in the following formula. The average molecular weight measured by gel permeation chromatography (using dimethyl sulfoxide as a solvent and polystyrene with a narrow molecular weight distrib...

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Abstract

The invention discloses a single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant as well as a preparation method and an application thereof. the preparation method comprises the following steps: at 90-110 DEG C, a nucleophilic substitution reaction is carried out between pentaerythritol and phosphorous oxychloride, and PEPA is obtained; a reaction between PEPA and cyanuric chloride is carried out at -5-10 DEG C for 3-6 hours, a reaction between a product and a diamine compound is carried out at 50-60 DEG C for 5-10 hours, and then a reaction between the product and the diamine compound is carried out at 90-110 DEG C for 5-10 hours; finally the single-component phosphor-nitrogen double-ring cage-shaped macromolecular intumescent flame retardant is obtained for flame retardant modification of polymers. Compared with the prior art, the prepared single-component macromolecular intumescent flame retardant has the advantages of high flame retardation efficiency, good compatibility with polymers, etc.; the intumescent flame retardant whose weight is 20-25 wt% of polypropylene can be added into the polypropylene for endowing the polypropylene with good flame retardation performance, and the intumescent flame retardant can be widely applied to the fields of internal and external decorative parts of automobiles, furniture and electric appliances, wires and cables, building material, etc.

Description

technical field [0001] The invention relates to a halogen-free flame retardant, in particular to a single-component phosphorus-nitrogen bicyclic cage macromolecular expansion flame retardant and its preparation method and application. Background technique [0002] Intumescent flame retardants (IFRs) are considered to be one of the most promising green flame retardants in the field of polymer flame retardants because of their advantages such as low smoke, low toxicity, and droplet suppression. Among the existing IFR systems, ammonium polyphosphate / pentaerythritol (APP / PER) is the most commonly used. When APP / PER is added to the polymer, it can play a good role in flame retardancy, smoke suppression and anti-droplet. However, PER is a polar small molecule, which has poor compatibility with the polymer matrix, is easy to migrate, and is easy to absorb moisture; the thermal stability of the APP / PER system is poor, the flame retardant efficiency is low, and the addition amount i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08L23/12
CPCC08G73/0644C08G73/065C08L23/12C08L2201/02C08L2201/22C08L79/04
Inventor 赖学军谢华理曾幸荣李红强唐霜
Owner SOUTH CHINA UNIV OF TECH
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