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Phosphorus nitrogen intumescent flame retardant and preparation method thereof

An intumescent flame retardant, phosphorus-nitrogen series technology, applied in the field of phosphorus-nitrogen intumescent flame retardant and its preparation, can solve the problems of easy hydrolysis and volatilization, and achieve the prevention of melting dripping phenomenon, good thermal stability, Good flame retardant effect

Inactive Publication Date: 2014-10-15
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the traditional phosphorus-based flame retardants are volatile and easy to hydrolyze

Method used

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  • Phosphorus nitrogen intumescent flame retardant and preparation method thereof
  • Phosphorus nitrogen intumescent flame retardant and preparation method thereof
  • Phosphorus nitrogen intumescent flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] First add 0.05mol of melamine, 0.15mol of phosphorous acid and 100ml of DMF into a 250ml three-neck flask equipped with a constant pressure titration funnel, a stirrer and a condensing reflux device, mechanically stir and heat to a temperature of 116°C, then the solution It is a milky white turbid liquid. After stirring evenly, 0.075mol of paraldehyde is added, and the color of the solution gradually turns yellow and gradually deepens. Heat preservation mechanical stirring for 36 hours, stop the reaction. Cool down to 50°C, take out the obtained product, cool it, filter, wash with water, and dry to a constant weight to obtain a yellow solid, which is the target product phosphorus nitrogen-based intumescent flame retardant {1-[4,6-bis(1-phosphono -ethylamino)triazine-2-amino]-ethyl}phosphonic acid dimelamine salt.

[0021] from figure 1 It can be seen that 702.02m / z is the molecular ion peak of the flame retardant molecule, which is the base peak. It can be shown that...

Embodiment 2

[0023] First add 0.1mol of melamine, 0.34mol of phosphorous acid and 200ml of DMF into a 500ml three-necked flask equipped with a constant pressure titration funnel, a stirrer and a condensing reflux device, mechanically stir and heat to a temperature of 116°C, at this time the solution It is a milky white turbid liquid. After stirring evenly, 0.16 mol of paraldehyde is added, and the color of the solution gradually turns yellow and gradually deepens. Keep warm and mechanically stir for 38 hours to stop the reaction. Cool down to 50°C, take out the obtained product, cool it, filter, wash with water, and dry to a constant weight to obtain a yellow solid, which is the target product phosphorus nitrogen-based intumescent flame retardant {1-[4,6-bis(1-phosphono -ethylamino)triazine-2-amino]-ethyl}phosphonic acid dimelamine salt.

Embodiment 3

[0025] First add 0.15mol of melamine, 0.48mol of phosphorous acid and 300ml of DMF into a 500ml three-necked flask equipped with a constant pressure titration funnel, a stirrer and a condensing reflux device, mechanically stir and heat to a temperature of 116°C, then the solution It is a milky white turbid liquid. After stirring evenly, 0.24mol of paraldehyde is added, and the color of the solution gradually turns yellow and gradually deepens. Heat preservation mechanical stirring for 40 hours, stop the reaction. Cool down to 50°C, take out the obtained product, cool it, filter, wash with water, and dry to a constant weight to obtain a yellow solid, which is the target product phosphorus nitrogen-based intumescent flame retardant {1-[4,6-bis(1-phosphono -ethylamino)triazine-2-amino]-ethyl}phosphonic acid dimelamine salt.

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Abstract

The invention relates to a phosphorus-nitrogen expanding type flame retardant and a preparation method thereof. The preparation method of the phosphorus-nitrogen expanding type flame retardant comprises the following steps of: (1), weighing melamine, paraldehyde and phosphorous acid material in a molar ratio of (1.0-1.2):(1.5-2.0):(3.0-3.6); (2), placing phosphorous acid and the melamine in a three-neck flask, adding DMF (Dimethyl Formamide), stirring, heating up to 110 DEG C to 120 DEG C, adding the paraldehyde after a milk white turbidity solution is uniformly stirred for gradually yellowing the solution, reacting for 36-48 hours, and stopping the reaction; (3), cooling to 50 DEG C to 60 DEG C, getting out the obtained product and cooling the product, filtering in suction and water-washing, and drying to the constant weight to obtain yellow powder solid, i.e., the phosphorus-nitrogen expanding type flame retardant. The phosphorus-nitrogen expanding type flame retardant has the following advantages of being rich in carbon source, acid source and gas source, good in thermal stability, high in nitrogen content and good in foaminess.

Description

technical field [0001] The invention relates to a phosphorus-nitrogen series intumescent flame retardant and a preparation method thereof. Background technique [0002] With the development of modern science and technology, in recent years, synthetic fibers, plastics, rubber and other polymer materials have been widely used in various fields, playing a huge role in the country's economic construction and people's lives. But for those polymer materials, they are generally all combustible or combustible, so just constituted a huge threat to people's life and property. [0003] Since the 1980s, flame retardants have become the largest additives used in synthetic materials next to plasticizers. Among flame retardants, although inorganic flame retardants are effective, they are added in relatively large amounts. Among the halogenated flame retardants, the brominated flame retardants are used in the largest amount, but they are prone to produce harmful substances during the comb...

Claims

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Application Information

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IPC IPC(8): C08K5/5353C07F9/6521C08L63/00
Inventor 黄齐茂朱宗民潘志权樊继亮
Owner WUHAN INSTITUTE OF TECHNOLOGY