Organic phosphinic acid metal salt containing triazine ring and preparation method thereof

The technology of metal phosphinic acid salt and triazine ring is applied in the field of metal organic phosphinic acid salt and its preparation, which can solve the problems of high molecular polarity, influence on flame retardant performance, decrease in mechanical properties of materials, etc., and achieve good dispersibility. , the molecular weight is large, the effect of improving the flame retardant performance

Active Publication Date: 2011-11-02
昆山卡帝德塑料制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the purity and yield of dialkyl phosphinates prepared by this method are high, the dialkyl phosphinates prepared by this method have small molecular weight and large molecular polarity, and are used as flame retardants in polymer materials. When the compatibility with the base material is poor, the mechanical properties of the material are seriously reduced, and only phosphorus is used as a flame retardant element, which cannot produce a synergistic effect, which affects the flame retardant performance.

Method used

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  • Organic phosphinic acid metal salt containing triazine ring and preparation method thereof
  • Organic phosphinic acid metal salt containing triazine ring and preparation method thereof
  • Organic phosphinic acid metal salt containing triazine ring and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Add 1188g of 50% hypophosphorous acid aqueous solution and 3L of acetic acid to a 10L three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, stir and heat to 90°C, and uniformly inject and dissolve 748g (3mol) of isocyanurate within 10h Acetate triallyl ester and 40g acetic acid solution of tert-butyl peroxy benzoate, control the reaction temperature not to exceed 95°C, and keep stirring for 1 hour after the injection of the solution is completed. Transfer the liquid in the flask to a 20L high-pressure reactor, seal it, exhaust the air in the reactor, heat to 90°C, feed ethylene, set the pressure to 0.6MPa through the pressure reducing valve on the ethylene cylinder, and set the pressure at a constant Pump 5% acetic acid solution of tert-butyl benzoate peroxide at a high speed, control the temperature in the reactor with cooling water to not exceed 95°C until the consumption of ethylene no longer increases, stop pumping the initiator...

Embodiment 2

[0038] Example 2 Add 954g (9mol) of sodium hypophosphite monohydrate and 3L of acetic acid into a 10L three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, stir and heat to 115°C, and uniformly inject and dissolve 785g (3.15mol) of sodium hypophosphite in 10 hours. ) acetic acid solution of triallyl isocyanurate and 50 g of benzoyl peroxide, control the reaction temperature not to exceed 120° C., and keep stirring for 1 hour after the injection of the solution is completed. Transfer the liquid in the flask to a 20L high-pressure reactor, seal it, exhaust the air in the reactor, heat it to 115°C, feed ethylene, set the pressure to 0.6MPa through the pressure reducing valve on the ethylene cylinder, and set the pressure at a constant Pump 5% benzoyl peroxide acetic acid solution at high speed, control the temperature in the reactor not to exceed 120°C with cooling water until the consumption of ethylene no longer increases, stop pumping the initiator ...

Embodiment 3

[0039]Example 3 Add 954g (9mol) of sodium hypophosphite monohydrate and 3L of acetic acid into a 10L three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, stir and heat to 100°C, and uniformly inject and dissolve 823g (3.3mol) of sodium hypophosphite in 10 hours. ) acetic acid solution of triallyl isocyanurate and 30 g of azobisisoheptanonitrile, the reaction temperature is controlled not to exceed 105° C., and the solution is kept for 1 hour after injection. Transfer the liquid in the flask to a 20L high-pressure reactor, seal it, exhaust the air in the reactor, heat it to 100°C, feed ethylene, and set the pressure to 0.6MPa through the pressure reducing valve on the ethylene cylinder, at a constant Pump in 5% azobisisoheptanonitrile acetic acid solution at high speed, control the temperature in the reactor not to exceed 105°C with cooling water until the consumption of ethylene no longer increases, stop pumping the initiator solution, keep the tem...

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Abstract

The invention relates to organic phosphinic acid metal salt containing a triazine ring and a preparation method thereof. The structure of the compound is represented as follows: FORMULA, wherein M is a metal ion of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Ce, Sn, Fe, Mn, Li, Na or K; and n is a valence of the M. The preparation method comprises the following steps of: reacting the phosphinic acid or alkali metal salt of the phosphinic acid with triallyl isocyanurate and ethylene in the presence of a radical initiator so as to obtain organic phosphinic acid or alkali metal salt of the organic phosphinic acid containing the triazine ring; and then, reacting with a metal compound of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Ce, Sn, Fe and Mn so as to obtain the relative organic phosphinic acid salt containing the triazine ring. The compound can be used as a fire retardant of nylon, polyester, polyurethane, epoxy resin, glass fibre reinforced resin, coat and the like. The preparation method is simple in process and easy to perform industrial production.

Description

Technical field: [0001] The invention relates to a metal salt of organic phosphinic acid containing a triazine ring and a preparation method thereof, in particular to a metal salt of a reaction product of triallyl isocyanurate, ethylene and hypophosphorous acid and a preparation method thereof. The compound can be used as a flame retardant for nylon, polyester, polyurethane, epoxy resin, glass fiber reinforced plastic resin, paint and other materials. Background technique: [0002] At present, due to the requirement of non-halogenation, organic phosphine flame retardants have become a research hotspot, especially organic phosphinic acid metal salt flame retardants are more popular because of their high flame retardant efficiency, small addition amount, non-toxic and environmentally friendly, and mechanical Good performance, high relative leakage index (CTI). More representative compounds are dialkylphosphinates, especially diethylphosphinates. Many preparation methods have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6521C08K5/5313C08L77/00C08L67/00C08L75/04C08L63/00C09D7/12
Inventor 王彦林纪孝熹
Owner 昆山卡帝德塑料制品有限公司
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