Novel fire retardant microencapsulated red phosphorus and preparation method thereof

一种微胶囊红磷、阻燃剂的技术,应用在新型阻燃剂微胶囊红磷及其制备领域,能够解决颗粒易团聚等问题

Inactive Publication Date: 2014-04-16
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the coating preparation of RP, the use of catalysts can improve the surface activity of RP and make it easier for organic resins to coat its surface. At present, there are many reports on the use of catalysts. Yang Fuxing [1] Sodium persulfate was used as a catalyst in a master's project, red phosphorus was coated with phenol-formaldehyde prepolymer, and the pH of the reaction solution was controlled to 8-9 to prepare microcapsule red phosphorus with good thermal stability. There is a disadvantage that the particles are easy to agglomerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Such as figure 1 As shown, weigh phenol, formaldehyde, and methanol with a mass ratio of 20:20:1, mix and add an appropriate amount of deionized water, control the reaction temperature at about 70 ℃, and add dropwise a NaOH solution with a molar concentration of 0.1 mol / L to adjust the pH , Keep the solution in a weakly alkaline environment with pH=8. After 25 minutes of reaction, a transparent solution is obtained, which is a phenol-formaldehyde prepolymer.

[0020] Weigh 10.0 g of ultra-fine red phosphorus (400 mesh), dissolve it in a proper amount of water, sonicate for 15 min, add 0.2 g of sodium lauryl sulfonate, stir well at 65 ℃, and then add 0.2 g of sodium persulfate, Then add 1.0 g of phenol-formaldehyde prepolymer and react for 0.5 h. In this process, adjust the pH to 2 with 0.1 mol / L HCL and 0.1 mol / L NaOH aqueous solution. After the reaction is completed, the solution is cooled, filtered, washed, and dried to obtain red phosphorus microcapsules coated with p...

Embodiment 2

[0022] Weigh phenol, formaldehyde, and methanol with a mass ratio of 20:28:1, mix and add an appropriate amount of deionized water, control the reaction temperature at about 75 ℃, and add dropwise NaOH solution with a molar concentration of 0.1 mol / L to adjust the pH to make the solution Always maintain a weak alkaline environment with pH = 8, and after 25 minutes of reaction, a transparent solution is obtained, which is a phenol-formaldehyde prepolymer.

[0023] Weigh 10.0 g of ultra-fine red phosphorus (400 mesh), dissolve it in an appropriate amount of water, ultrasonically treat it for 15 minutes, add 0.2 g of sodium hexametaphosphate, stir well at 65 ℃, then add 0.2 g of ammonium persulfate, and then add 1.5 g phenol-formaldehyde prepolymer, react for 1 h. During this process, adjust the pH to 6 with 0.1 mol / L NaOH and 0.1 mol / L NaOH aqueous solution. After the reaction is completed, the solution is cooled, filtered, washed, and dried to obtain red phosphorus microcapsules ...

Embodiment 3

[0025] Weigh phenol, formaldehyde, and methanol with a mass ratio of 20:20:1, mix and add an appropriate amount of deionized water, control the reaction temperature at about 80 ℃, and add dropwise NaOH solution with a molar concentration of 0.1 mol / L to adjust the pH to make the solution Always maintain a weak alkaline environment with pH = 8.5. After 35 minutes of reaction, a transparent solution is obtained, which is a phenol-formaldehyde prepolymer.

[0026] Weigh 10.0 g of ultra-fine red phosphorus (800 mesh), dissolve it in a suitable amount of water, ultrasonically treat it for 20 min, add 0.1 g of polyethylene glycol 200, stir well at 65 ℃, then add 0.3 g of ammonium persulfate, and then add 1.0 g of phenol-formaldehyde prepolymer was reacted for 1.5 h. During this process, adjust the pH to 4 with 0.1 mol / L HCL and 0.1 mol / L NaOH aqueous solution. After the reaction is completed, the solution is cooled, filtered, washed, and dried to obtain red phosphorus microcapsules co...

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PUM

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Abstract

The invention discloses a novel fire retardant microencapsulated red phosphorus which is formed by wrapping phenol-formaldehyde prepolymer (PFP) on the surface of superfine red phosphorus powder. Due to addition of a high-efficient catalyst in the preparation process, the surface activity of the red phosphorus is improved, the surface of the red phosphorus is tightly wrapped with a PFP layer, and meanwhile as methanol is added to prevent formaldehyde auto-agglutination and the pH value of a reaction solution in the wrapping process is controlled to be 1-6, the stability and the resistivity of the red phosphorus are improved, the machining property is improved, and meanwhile the moisture absorption rate and the PH3 release amount are greatly reduced.

Description

technical field [0001] The invention relates to a novel flame retardant microcapsule red phosphorus and a preparation method thereof, belonging to the field of chemical preparation. technical background [0002] With the enhancement of people's awareness of environmental protection, the impact of flame retardant products on the environment has become the first consideration in choosing flame retardants. For a long time, halogenated flame retardants have been one of the important flame retardants, but due to the release of toxic fumes when they burn, causing secondary hazards, they have been gradually restricted or even replaced. [0003] Red phosphorus (red phosphorus, RP) is a highly efficient halogen-free and environmentally friendly flame retardant, but ordinary RP, especially ultra-fine RP, has serious stability and safety problems in the preparation, storage and production processes, low ignition point, The problems of spontaneous combustion, explosive dust, easy moist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K3/02C08G8/10C08L101/00
Inventor 刘孝恒杨福兴刘山杨小燕蒋文俊
Owner NANJING UNIV OF SCI & TECH
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