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Calcined kaolin-based composite flame retardant for epoxy resin and its preparation and application

A technology of compound flame retardant and calcined kaolin, applied in the field of flame retardant, can solve the problems of inability to withstand high temperature, difficult to mix uniformly, low decomposition temperature, etc. Effect

Active Publication Date: 2021-12-17
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis of ammonium polyphosphate usually requires high temperature and high pressure, the process is complicated, the cost is high, and the decomposition temperature is low, it cannot withstand high temperature, and it is difficult to mix evenly when it is simply compounded with layered silicate

Method used

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  • Calcined kaolin-based composite flame retardant for epoxy resin and its preparation and application
  • Calcined kaolin-based composite flame retardant for epoxy resin and its preparation and application
  • Calcined kaolin-based composite flame retardant for epoxy resin and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] According to the mass ratio of 1.8:1, take calcined kaolin and 85wt% phosphoric acid solution respectively, and then take powdered urea, the mass ratio of urea and phosphoric acid contained in phosphoric acid solution is 1:1; add calcined kaolin and phosphoric acid solution with In a three-necked flask with a reflux condenser and an electric stirrer, slowly heat to 75°C under mechanical stirring, and keep warm for 5 hours to obtain a mixture S1; add urea to the mixture S1 and stir thoroughly until the urea is completely dissolved to obtain a uniform mixture S2; Heat the mixture S2 to 100°C at a heating rate of 1°C / min. After the mixture S2 becomes thick and viscous, stop heating and keep it warm for 5 minutes to obtain the product; put the product in a vacuum oven, cure it at 180°C for 5 hours, and take it out. Cool to room temperature and grind to obtain a calcined kaolin-based composite flame retardant for epoxy resin.

[0032] Use silane coupling agent (KH-550) to mo...

Embodiment 2

[0034] According to the mass ratio of 1.8:1, take calcined kaolin and 85wt% phosphoric acid solution respectively, and then take powdered urea, the mass ratio of urea and phosphoric acid contained in phosphoric acid solution is 1:1; add calcined kaolin and phosphoric acid solution with In a three-necked flask with a reflux condenser and an electric stirrer, slowly heat to 95°C under mechanical stirring, and keep warm for 0.5h to obtain a mixture S1; add urea to the mixture S1, and stir well until the urea is completely dissolved to obtain a uniform mixture S2; Heat the mixture S2 to 150°C at a heating rate of 5°C / min. After the mixture S2 becomes thick and viscous, stop heating and keep it warm for 10 minutes to obtain the product; put the product in a vacuum oven and cure it at 250°C for 1 hour, and take it out , cooled to room temperature, and ground to obtain a calcined kaolin-based composite flame retardant for epoxy resin.

[0035] Use silane coupling agent (KH-560) to mo...

Embodiment 3

[0037] According to the mass ratio of 1.8:1, take calcined kaolin and 85wt% phosphoric acid solution respectively, and then take powdered urea, the mass ratio of urea and phosphoric acid contained in phosphoric acid solution is 1:1; add calcined kaolin and phosphoric acid solution with In a three-necked flask with a reflux condenser and an electric stirrer, slowly heat to 85°C under mechanical stirring, and keep it warm for 2.7 hours to obtain a mixture S1; add urea to the mixture S1 and stir thoroughly until the urea is completely dissolved to obtain a uniform mixture S2; The temperature of the mixture S2 was raised to 125°C at a heating rate of 3°C / min. After the mixture S2 became thick and viscous, the heating was stopped and the product was kept for 7.5 minutes to obtain the product; the product was put into a vacuum oven and cured at 215°C for 3 hours. Take it out, cool to room temperature, and grind to prepare a calcined kaolin-based composite flame retardant for epoxy resi...

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Abstract

The invention discloses a calcined kaolin-based composite flame retardant for epoxy resin and its preparation and application. The composite flame retardant uses calcined kaolin particles as a basic component, and ammonium polyphosphate produced by in-situ polymerization is formed on the surface of kaolin and Kaolin combines to form a composite structure. Using phosphoric acid and urea as raw materials, the composite flame retardant was prepared by in-situ polymerization on the surface of calcined kaolin. Adding it to epoxy resin can improve the flame retardant performance of epoxy resin, effectively reduce the thermal weight loss rate and heat release rate of epoxy resin, and improve its carbon residue and carbon density. The preparation method of the present invention is simple and easy to operate, low in cost, and ingenious in preparation ideas. Through in-situ polymerization, kaolin and ammonium polyphosphate produced by in-situ polymerization are closely and uniformly combined. The composite flame retardant has the characteristics of halogen-free, high efficiency, and environmental friendliness. The scope of application of kaolin and epoxy resins.

Description

technical field [0001] The invention belongs to the field of flame retardant technology, and relates to a composite flame retardant, in particular to a calcined kaolin-based composite flame retardant for epoxy resin, and also relates to a preparation method and an application method of the composite flame retardant. Background technique [0002] As one of the most widely used polymers, epoxy resin (EP) has many excellent physical and chemical properties, and is widely used in coatings, adhesives, biomedicine, composite materials, electronic devices, aerospace and other fields. Among them, the most widely used and the largest output is glycidyl ether type epoxy resin, which is formed by polycondensation of bisphenol A and epichlorohydrin. It is generally considered to be this type of epoxy resin. The typical resin bisphenol A diglycidyl ether (DGEBPA) structure such as figure 1 shown. The limiting oxygen index of ordinary EP is only 19%, which is easy to burn and cause fire...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K3/34C08K3/32C08K9/06C08L63/00
CPCC08K3/346C08K3/32C08K9/06C08L2201/02C08L2201/22C08K2003/323C08L63/00
Inventor 王育华马俊吴秋荣肖奇
Owner LANZHOU UNIVERSITY
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