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Preparation method and application of three-source integrated hyperbranched structure flame retardant

A structural flame retardant, hydroxyl-terminated hyperbranched technology, applied in the field of flame retardant preparation, can solve the problems of low molecular weight, weakened material mechanical properties, poor polymer compatibility, etc., achieve good fluidity, improve mechanical properties, etc. performance effect

Active Publication Date: 2017-05-10
东莞市震亚精密技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the "three sources in one" intumescent flame retardant is mainly composed of small molecules as acid source, carbon source and gas source, such as phosphorus oxychloride (or phosphoric acid), melamine and pentaerythritol, which are obtained by the mutual reaction, and the molecular weight of the obtained product is not large. , poor compatibility with polymers, and the presence of small molecules tends to weaken the mechanical properties of materials

Method used

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  • Preparation method and application of three-source integrated hyperbranched structure flame retardant
  • Preparation method and application of three-source integrated hyperbranched structure flame retardant
  • Preparation method and application of three-source integrated hyperbranched structure flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Preparation of reactive "three sources in one" hyperbranched structure flame retardant

[0021] Step 1. Add the hydroxyl-terminated hyperbranched polyester and phosphoric acid into the reactor, and add the catalyst phosphotungstic acid or p-toluenesulfonic acid. The molar ratio of the hydroxyl-terminated hyperbranched polyester, phosphoric acid, and catalyst is 1:0.4:0.5 %;

[0022] Step 2, heating up to 80°C, and reacting under vacuum for 4 hours;

[0023] Step 3, wash with ethanol, after drying, dissolve in acetone;

[0024] Step 4: After adding ethylenediamine in an equimolar ratio to phosphoric acid and reacting for 30 minutes, the precipitate was obtained, washed three times with ethanol, and dried to obtain a light yellow powder, which is a reactive "three sources in one" hyperbranched structure flame retardant.

[0025] The reaction equation of the reactive "three sources in one" hyperbranched structure flame retardant is as follows:

[0026]

[0...

Embodiment 2

[0032] Example 2 Application of reactive "three sources in one" hyperbranched structure flame retardant

[0033] The reactive "three sources in one" hyperbranched structure flame retardant can be used as a chain extender or crosslinking agent in the polyurethane reaction system, becoming a reactive "three sources in one" flame retardant in the polyurethane system. The specific operation steps are as follows:

[0034] Mix partially flame-retardant modified hyperbranched polyester with polyester polyol and toluene diisocyanate in a certain proportion, add catalyst triphenylbismuth, mix well, defoam, put into mold and cure at 60°C for 2 days. Wherein, the polyester polyol of this embodiment can also be replaced with other polyols, such as polyether polyols, polybutadiene polyols and other polyurethane raw materials; toluene diisocyanate can also be other polyisocyanates.

[0035] Taking the fourth-generation hydroxyl-terminated hyperbranched polyester as an example, the polyuret...

Embodiment 3

[0039] Example 3 Application of Reactive "Three Sources in One" Hyperbranched Structure Flame Retardant

[0040] The reactive "three sources in one" hyperbranched structure flame retardant can react with monomers containing double bonds (such as acrylic acid, oleic acid, etc.), and can obtain end groups containing double bonds, which can be used as reactive type of olefin polymer materials "Three sources in one" flame retardant. Taking the modified part of acrylic acid as an example, the reaction equation is as follows:

[0041]

[0042] The specific preparation method is as follows:

[0043]The flame-retardant modification of part of the end group of the hydroxyl-terminated hyperbranched polyester is obtained to obtain a reactive "three sources in one" hyperbranched structure flame retardant. In the Boltorn type hyperbranched polyester, the hydroxyl group of the y part that does not participate in the reaction reacts with the carboxylic acid containing double bonds to ob...

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Abstract

The invention discloses a preparation method of a three-source integrated hyperbranched structure flame retardant. The preparation method of the three-source integrated hyperbranched structure flame retardant comprises the following steps: 1, adding hydroxyl terminated hyperbranched polyester and phosphoric acid into a reactor, and further adding a catalyst, namely phosphotungstic acid or p-toluenesulfonic acid; 2, heating to the temperature of 80 DEG C, and reacting for 4 hours under a vacuum condition; 3, washing with ethanol, and dissolving in acetone after drying; 4, adding ethylenediamine of which the molar ratio is equal to that of phosphoric acid to be reacted for 30 minutes, obtaining a precipitate, washing with ethanol for 3 times, and drying to obtain light yellow powder. The flame retardant obtained by adopting the method is mixed with acrylic acid, PP and the like, so that polyurethane flame-retardant PP with low viscosity and high mechanical properties can be obtained. The invention further discloses application of the three-source integrated hyperbranched structure flame retardant used as a polymer material.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation, and in particular relates to a preparation method and application of a "three sources in one" hyperbranched structure flame retardant. Background technique [0002] Intumescent flame retardant technology is a new type of flame retardant technology developed in the mid-1990s. In the case of intumescent flame retardant (IFR) flame retardant plastics, an intumescent carbon layer will form on the surface of the plastic, which plays the role of heat insulation, oxygen insulation, smoke suppression and prevention of melting droplets, and has low smoke, low toxicity, no melting droplets, and no Corrosive gases are produced. Phosphorus-nitrogen IFR is a composite flame retardant mainly composed of phosphorus, nitrogen, and carbon. It is mainly composed of three parts: (1) acid source, also known as carbonization catalyst or dehydrating agent, usually inorganic acid compound or inorga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G18/42C08L67/00C08L23/12
Inventor 宋雪晶
Owner 东莞市震亚精密技术有限公司
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