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Bisphenol A(phenyl polyphosphoric acids easter) flame retardant and preparation thereof

A technology of polyphosphate and flame retardant, applied in the direction of fire retardant coatings, etc., can solve the problems of reduced flame retardant effect, poor product surface quality, poor compatibility, etc., and achieve the effect of improving impact strength and ensuring flame retardant effect

Active Publication Date: 2010-12-08
雅克(上海)化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet BDP is said as Chinese patent 00808793.8, 00808793.84, is a relatively small liquid product of a kind of molecular weight (mainly the mixture of single molecule, and a small amount of dimer and very little trimer), and the resin miscibility with large molecular weight is relatively Poor, the added resin is prone to migrate to the surface during molding, resulting in the so-called "juicing", this migration is more likely to occur when the temperature is higher
The migration of flame retardants will not only cause the surface quality of the product to deteriorate, but also reduce the flame retardant effect, and the overflowing BDP will also cause environmental pollution; secondly, due to poor compatibility, it will cause the resin to bend when used in the resin The mechanical properties such as modulus, tensile strength, deflection temperature, and impact resistance are reduced, and the processability will also be deteriorated

Method used

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  • Bisphenol A(phenyl polyphosphoric acids easter) flame retardant and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The first step is the synthesis of intermediate monomers: 460g phosphorus oxychloride (POCl 3 ) Put into a four-neck flask with stirring and thermometer, add a small amount of Lewis acid catalyst, stir and heat to about 100℃, add 228g of bisphenol A in batches, keep the temperature for 3-4 hours, and collect the hydrogen chloride produced by the reaction Gas (such as water absorption), gradually increase the temperature to reflux and continue the reaction for 2 hours, until no HCl escape is detected (the reaction ends). Distill out unreacted POCl under reduced pressure 3 , 462g of intermediate product monomer was obtained.

[0019] The second step of polycondensation: Put 210g of bisphenol A into the prepared intermediate monomer at 110°C in batches, react for 3-4 hours, collect the hydrogen chloride gas produced by the reaction, raise the temperature to 140-150°C, and continue the reaction for 3 hours Above, until no HCl escape is detected (reaction equilibrium), 639 g of...

Embodiment 2

[0022] Example 2: Same as Example 1. After the intermediate product monomer is obtained by the reaction in the first step, double the amount of xylene solvent of the intermediate product monomer is added, and the second, third, and fourth steps are followed. The obtained solid flame-retardant resin has an average molecular weight of 6,500.

Embodiment 3

[0023] Example 3: Same as Example 1. After the intermediate product monomer is obtained by the reaction in the first step, 1.5 times the amount of triethyl phosphate (TEP) solvent is added to the intermediate product monomer, and then the second, third, and fourth steps are followed. At the same time, the reaction temperature in the second step was increased to 155-165°C. The obtained solid flame-retardant resin has an average molecular weight of 10,500.

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Abstract

The present invention provides an improvement towards bisphenol A double (diphenyl phosphate) flame retardant and a preparation and is characterized in that medium product monomer is obtained by the condensation reaction of excessive phosphorus oxychloride and the bisphenol A; the unreacted phosphorus oxychloride is removed; the medium product monomer is continuously processed for the polycondensation reaction with the bisphenol A till to balance to obtain multimer; chlorine atom at the multimer is replaced by excessive phenol to obtain solid macromolecular flame retarding polymer with the molecular weight of 2300 to 13000, and n is equal to 5 minus 40. The bisphenol A double (diphenyl phosphate) flame retardant obtained by the present invention not only has the flame retarding performance which is similar as BDP, the bisphenol A double (diphenyl phosphate) flame retardant but also has very good solubility with resin and does not fluid easily after being added into the resin, so the present invention does not cause the transfer of press juice and can ensure the flame retarding effect; the present invention can also improve the impact intensity, thermal deformation temperature, pull intensity, elongation rate, bending strength, bending modulus and fluidity (process) of flame retarding resin and accordingly conquers the disadvantage brought by using liquid BDP.

Description

Technical field [0001] The present invention is an improvement of bisphenol A bis(diphenyl phosphate) flame retardant, and particularly relates to a solid resin type bisphenol A (phenyl polyphosphate) flame retardant and its preparation. Background technique [0002] Bisphenol A bis(diphenyl phosphate) flame retardant (hereinafter referred to as BDP), with low volatility, is a well-known flame retardant used in flammable resins, especially for polycarbonate / acrylonitrile- The butadiene-styrene copolymer (PC / ABS) composition has better flame retardant effect. Its synthesis is by excess phosphorus oxychloride (POCl 3 ) Condensation reaction with bisphenol A to obtain the intermediate product monomer, and then react with phenol to replace the chlorine atoms at both ends to obtain BDP. However, BDP, as stated in Chinese patents 00808793.8 and 00808793.84, is a liquid product with a relatively small molecular weight (mainly a single molecule, and a mixture of a small amount of dimers...

Claims

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Application Information

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IPC IPC(8): C09K21/14C08G79/04
Inventor 沈琦周乐群仇国才周荣生吴仁铭
Owner 雅克(上海)化工新材料有限公司
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