Method for preparing phosphor modified flame retardation stiffening agent

A hardener, phosphorus-modified technology, applied in the field of flame-retardant and heat-resistant phosphorus-modified flame-retardant hardeners, which can solve low curing density, reduced gelling or hardening density, thermal properties and adhesion properties Variation etc.

Active Publication Date: 2010-12-29
KANGNAM CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, conventional non-halogen-based flame retardant hardeners have the following problems: a large amount of phosphorus raw material is introduced to impart favorable flame retardancy to the epoxy molecular structure, resulting in gelation or decrease in hardened density due to increased molecular weight
Therefore, the cured product has the disadvantage that inherent physical properties such as heat resistance, adhesiveness, thermal stability, etc. are drastically deteriorated
In other words, although the reaction by a large amount of phosphorus-based raw materials is sufficient to ensure flame retardancy, a compound with a relatively large molecular structure is produced, resulting in steric hindrance effects and low curing density
As a result, thermal properties and adhesion properties deteriorate

Method used

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  • Method for preparing phosphor modified flame retardation stiffening agent
  • Method for preparing phosphor modified flame retardation stiffening agent
  • Method for preparing phosphor modified flame retardation stiffening agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0148] 228g (1 mole) of bisphenol A, 216g (3 moles) of paraformaldehyde, 30g of water and 10g of 50% aqueous sodium hydroxide solution were placed in a reaction bath, and then reacted at 50° C. for 5 hours under heating and stirring. Next, after adding 100 g of water thereto, neutralization was performed with 5 g of 0.1N sulfuric acid. The product was then washed three times with 100 g of water to separate and obtain a bisphenol A resol compound (304.3 g, yield 94.8%). This resole phenolic resin compound was added to 610 g of methanol, and the resole phenolic resin compound was subjected to alcoholysis at 70° C. (T) for 5 hours with stirring. Thereafter, 522.15 g (2.417 mol) of DOPO was added to the mixture, and dealcoholysis was performed at 145° C. (T) for 10 hours under heating and stirring while removing the methanol portion. After the reaction was completed, the remaining water and methanol were removed under vacuum or reduced pressure, thereby obtaining 749 g of a phosp...

Embodiment 2

[0151] 228g (1 mole) of bisphenol A, 108.4g (1.5 moles) of paraformaldehyde, 30g of water and 5g of 50% aqueous sodium hydroxide solution were placed in a reaction bath, and then reacted at 50°C for 5 hours under heating and stirring. Next, after adding 76 g of water thereto, neutralization was performed with 2.5 g of 0.1N sulfuric acid. The product was then washed three times with 76 g of water to separate and obtain a bisphenol A resol compound (260.6 g, yield 95%). This resole phenolic resin compound was added to 521 g of methanol, and the resole phenolic resin compound was subjected to alcoholysis at 70° C. (T) for 5 hours with stirring. Thereafter, 261.6 g (1.211 mol) of DOPO was added to the mixture, and dealcoholysis was performed at 145° C. (T) for 10 hours under heating and stirring while removing the methanol portion. After the reaction was completed, the remaining water and methanol were removed under vacuum or reduced pressure, thereby obtaining 460 g of a phospho...

Embodiment 3

[0154] 228g of bisphenol A, 288.4g (4 moles) of paraformaldehyde, 30g of water and 14g of 50% aqueous sodium hydroxide solution were placed in a reaction bath, and then reacted at 50° C. for 5 hours under heating and stirring. Next, after adding 116 g of water thereto, neutralization was performed with 6.7 g of 0.1N sulfuric acid. The product was then washed three times with 116 g of water to separate and obtain bisphenol A resol compound (323 g, yield 92%). This resole phenolic resin compound was added to 646 g of methanol, and the resole phenolic resin compound was subjected to alcoholysis at 70°C (T) for 5 hours with stirring. Thereafter, 675.6 g (3.128 mol) of DOPO was added to the mixture, and dealcoholysis was performed at 145° C. (T) for 10 hours under heating and stirring while removing the methanol portion. After the reaction was completed, the remaining water and methanol were removed under vacuum or reduced pressure, thereby obtaining 883 g of a phosphorus-modified...

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PUM

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Abstract

The invention discloses a method for preparing a phosphor modified flame retardation stiffening agent with excellent flame resistance and hear resistance. The prepared flame retardation stiffening agent has excellent flame resistance, hear resistance, physical properties and chemical properties, so the stiffening agent is sufficient for being used as polycarbonate or an additive of other engineering plastics such as acrylonitrile-butadiene-styrene (ABS) and high impact polystyrene (HIPS), and also used as raw material of epoxy resin, cyanate resin and acrylate resin and/or a stiffening agent of the epoxy resin. Especially the flame retardation stiffening agent can be applied to highly reliable electrical/electronic elements such as insulating material of EMC, and various composite materials such as printed circuit board (PCB) base material and insulation plate which need excellent flame resistance and thermal stability, adhesive, coating agent, paint and the like.

Description

technical field [0001] The present invention relates to a method for preparing a phosphorus-modified flame-retardant hardener, more specifically, to a method for preparing a phosphorus-modified flame-retardant hardener with excellent flame retardancy and heat resistance. Background technique [0002] Plastics are currently used in many industrial applications including, for example, electrical equipment, transportation devices, construction materials, and the like. However, plastics containing carbon, oxygen, hydrogen, and the like are easy to burn, and thus it is particularly necessary to improve flame retardancy in consideration of safety in case of fire. [0003] In general, fire requires fuel, oxygen, and energy, and if any of these requirements are not met, no fire will start. That is, methods of flame retarding plastics may include eliminating at least one of such necessary parameters. The flame retardant hardener refers to a substance that delays ignition or combust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G8/04
Inventor 崔春求崔捀求李垠龙文璟明崔敬泰韩广洙
Owner KANGNAM CHEM
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