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Higher molecular weight type intumescent flame retardant containing triazine structure and synthetic method thereof

An intumescent flame retardant and high molecular weight technology, applied in the field of intumescent flame retardants, can solve the problems of compatibility, thermal stability to be further improved, low molecular weight, etc., to maintain the original performance, high molecular weight, use safe effect

Inactive Publication Date: 2013-05-15
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phosphorus-nitrogen intumescent flame retardants synthesized by these two methods integrate acid source, gas source and carbon source, but the molecular weight is low, and the compatibility with the matrix and thermal stability need to be further improved.

Method used

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  • Higher molecular weight type intumescent flame retardant containing triazine structure and synthetic method thereof
  • Higher molecular weight type intumescent flame retardant containing triazine structure and synthetic method thereof
  • Higher molecular weight type intumescent flame retardant containing triazine structure and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1: Phosphorus oxychloride reacts with pentaerythritol to obtain oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2,2,2]octane (PEPA).

[0030] In a 250ml three-neck flask equipped with a thermometer, a constant pressure funnel, and a reflux condenser, add 0.25mol of pentaerythritol and 0.425mol of dioxane solvent, raise the temperature to 80°C, and dropwise add 0.25mol of phosphorus oxychloride in 2 hours. The temperature was raised to 100°C, and the reaction was carried out with nitrogen gas for 4 hours. Stand still, cool, precipitate white crystals, and filter with suction. Wash with 0.5 mol of dioxane and 1 mol of absolute ethanol respectively. Vacuum dry at 70°C for 12h.

[0031] The second step: PEPA reacts with cyanuric chloride to obtain a substituted product of cyanuric chloride.

[0032] 0.033mol PEPA is dissolved in 0.031mol acetonitrile, and 0.033mol cyanuric chloride is dissolved in 0.046mol acetonitrile. PEPA and acetonitrile solution and 0.05mol ...

Embodiment 2

[0036] Step 1: Phosphorus oxychloride reacts with pentaerythritol to obtain oxo-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo[2,2,2]octane (PEPA).

[0037] In a 250ml three-neck flask equipped with a thermometer, a constant pressure funnel, and a reflux condenser, add 0.3mol of pentaerythritol and 0.425mol of dioxane solvent, raise the temperature to 85°C, add 0.25mol of phosphorus oxychloride dropwise in 4 hours, and raise the temperature to 105 ℃, reacted with nitrogen gas for 6h, let stand, cooled, precipitated white crystals, filtered with suction, washed with 0.5mol dioxane and 1mol anhydrous ethanol respectively, and dried in vacuum at 70°C for 12h to obtain oxo-4-hydroxymethyl- 2,6,7-Trioxa-1-phosphabicyclo[2,2,2]octane (PEPA), molecular weight 179.98.

[0038] Infrared data: wave number 3410cm -1 The -OH absorption peak is at 2970cm -1 at -CH 2 - Absorption peak, 1301cm -1 The place is P=O absorption peak, 1022cm -1 and 990cm -1 Nearby is the P-O-C absorption pea...

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Abstract

The invention discloses a higher molecular weight type intumescent flame retardant containing triazine structure and a synthetic method thereof. The higher molecular weight type intumescent flame retardant is a phosphorus / nitrogen intumescent flame retardant, which is free from halogen and toxicity, is safe in use and environmentally-friendly. The phosphorus / nitrogen intumescent flame retardant integrates an acidic source, a gas source and a carbon source; the triazine structure and a poly-benzene ring structure are introduced, so that high thermal stability is gained, the carbonizing capacity is high, and additive amount is low; and the phosphorus / nitrogen intumescent flame retardant is high in compatibility respect to a substrate, and can be used for avoiding moisture absorption and separation of the flame retardant, and remaining the original performances of the material to the maximum.

Description

technical field [0001] The invention belongs to the technical field of intumescent flame retardants. Specifically, the invention relates to a large molecular weight intumescent flame retardant containing a triazine structure and a synthesis method thereof. Background technique [0002] Polymer materials are widely used for their light weight, corrosion resistance, and good insulation. However, polymer materials contain a large amount of hydrocarbon structure and are combustible and combustible materials. Therefore, since the 1980s, a large number of flame retardants have been added to various polymer materials in order to endow them with flame retardancy, self-extinguishing properties or smoke suppression properties. [0003] At present, flame retardants mainly include organohalogen, organophosphorus, inorganic, and nitrogen-phosphorus synergistic expansion systems. Organic halogen flame retardants are widely used and effective, but the combustion of such materials will pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C08L71/10
Inventor 徐卫兵朱道吉周正发任凤梅马海红
Owner HEFEI UNIV OF TECH
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