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Phosphorus nitrogen composite flame retardant and preparation method thereof

A flame retardant and composite technology, applied in the field of phosphorus-nitrogen composite flame retardant with ester group and its preparation, can solve the problem of uniform dispersion of resin substrate, poor thermal stability of pentaerythritol, loss of practical use value, etc. It can solve the problem of poor heat resistance, good dispersibility and easy industrial production.

Active Publication Date: 2014-10-22
应急管理部四川消防研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most mature and widely used intumescent flame retardant is the classic intumescent flame retardant system: ammonium polyphosphate + pentaerythritol (+ melamine), but the phosphorus nitrogen composite flame retardant composed of ammonium polyphosphate + pentaerythritol (+ melamine) There are still many application defects in the flame retardant, mainly as follows: (1) The three components are all compounds that cannot be melted at the processing temperature of most flame retardant materials, or thermal decomposition or sublimation begins near the melting point of these materials, making the flame retardant The temperature window of the melt processing of the agent itself is too narrow, and the uniform dispersion in the resin base material becomes difficult, resulting in a great reduction in the mechanical properties of the material, which even cannot meet the standard requirements, and loses the actual use value; (2) The thermal stability of pentaerythritol is poor, and the initial heat The decomposition temperature is 211°C, and it is easy to decompose at the processing temperature of many polymers
In response to the above problems, relevant researchers have carried out a lot of research work, but so far, there have been no reports on phosphorus-nitrogen composite flame retardants with good thermal stability and melting properties.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 800g of tris(2-hydroxyethyl)isocyanurate (THEIC), 26.5g of 9,10-dihydro-9-oxa-10-phosphophenanthrene-succinic acid (DDP), 241.6g Terephthalic acid and 4g of tetrabutyl titanate were added to the reaction kettle, filled with nitrogen to remove the air in the kettle, and pressurized to 0.07MPa; under mechanical stirring, the temperature was raised to 200-240°C within 2 hours to carry out the esterification reaction, and the inside of the kettle was controlled. The pressure is ≤0.1MPa. When the water generated by the esterification reaches 50ml, the esterification reaction is over; vacuum dehydration reaction at 230-245°C for 0.5-1.5h, add 152g molecular sieve, stir evenly and then discharge. The resulting product has a melting point of 75-80°C and an initial thermal decomposition temperature of 246°C.

[0051] After the above product was pulverized and finely passed through a 100-mesh sieve, 230 g was mixed with 770 g of ammonium polyphosphate with a polymerization degree...

Embodiment 2

[0053] Add 800g THEIC, 150.4g of DDP, 288.7g of terephthalic acid and 4.5g of tetrabutyl titanate into the reaction kettle, fill with nitrogen to remove the air in the kettle, pressurize to 0.07MPa; heat up to 0.07MPa within 2h under mechanical stirring Carry out the esterification reaction at 200-240°C, and control the pressure in the kettle to ≤0.1MPa. When the water generated by the esterification reaches 70ml, the esterification reaction is over; vacuum dehydration reaction at 230-245°C for 0.5-1.5h, add 115.4g molecular sieve , and discharge after stirring evenly. The resulting product has a melting point of 110-116°C and an initial thermal decomposition temperature of 265°C.

[0054] After the above product was pulverized and finely passed through a 100-mesh sieve, 355 g was mixed with 645 g of silane-coated ammonium polyphosphate with a degree of polymerization ≥ 700 and mixed evenly in a high-speed mixer to obtain a phosphorus-nitrogen composite flame retardant (B). T...

Embodiment 3

[0056] Add 800g THEIC, 317.5g of DDP, 152.3g of terephthalic acid and 5g of antimony trioxide into the reaction kettle, fill with nitrogen to remove the air in the kettle, pressurize to 0.07MPa; raise the temperature to 200~200 within 2 hours under mechanical stirring Carry out the esterification reaction at 240°C, and control the pressure in the kettle to be ≤0.1MPa. When the water generated by the esterification reaches 60ml, the esterification reaction is over; vacuum dehydration reaction at 230-245°C for 0.5-1.5h, add 401g nano-montmorillonite Soil, stir evenly and discharge. The resulting product has a melting point of 92-97°C and an initial thermal decomposition temperature of 245°C.

[0057] After the above product was pulverized and finely passed through a 100-mesh sieve, 400 g was mixed with 600 g of epoxy resin-coated ammonium polyphosphate with a polymerization degree ≥ 700 and mixed evenly in a high-speed mixer to obtain a phosphorus-nitrogen composite flame retard...

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Abstract

The invention discloses a phosphorus-nitrogen compound fire retardant which is formed by mixing the following components: 20-97% of a reaction product of phosphorus-containing diacid and nitrogen containing triol or reaction product of phosphorus-containing diacid, nitrogen containing triol and aromatic dicarboxylic acid, 3-10% of a flame retardant synergist and 0-77% of ammonium polyphosphate. The invention also discloses a preparation method of the phosphorus-nitrogen compound fire retardant. Melting point of the adopted reaction product of phosphorus-containing diacid and nitrogen containing triol or the reaction product of phosphorus-containing diacid, nitrogen containing triol and aromatic dicarboxylic acid is low, initial thermal decomposition temperature is high, and the fire retardant has unique melting characteristic. Thus, appropriate melting processing temperature window of the fire retardant is wide, the gap that there is no phosphorus-nitrogen compound fire retardant which has good heat stability and melting characteristic at present is filled, and application range of the fire retardant is enlarged. The preparation method is mature and simple, is convenient to operate and easy to control, and is convenient for industrial production.

Description

technical field [0001] The invention belongs to the technical field of phosphorus nitrogen flame retardant and its preparation. Specifically, the invention relates to a class of phosphorus-nitrogen composite flame retardants with ester groups and a preparation method thereof. Background technique [0002] In recent years, fire accidents have occurred frequently, especially in public places and densely populated places. Once a fire accident occurs, it will not only cause property losses, but also cause heavy casualties. Therefore, the prevention of fire has attracted widespread attention. However, plastics, rubber, and synthetic fibers, which are widely used in various sectors of the national economy such as industry, agriculture, and military affairs, and their products, are mostly flammable and combustible items, not only have a large heat release rate when burning, High calorific value, fast flame propagation, difficult to extinguish, and sometimes produce dense smoke an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5313C08K5/5398C08K9/10C08K3/32C07F9/6571
Inventor 葛欣国刘微张翔李风卢国建兰彬刘军军彭波唐勇张帆张秉浩
Owner 应急管理部四川消防研究所