Melamine cyanurate derivative covalent triazine framework flame retardant, preparation method and application thereof

A technology of melamine cyanurate and melamine cyanurate, which is applied in the field of melamine cyanurate derivative covalent triazine frame flame retardant and its preparation, can solve the problems affecting the compatibility of epoxy resin, Problems such as the decline in the mechanical properties of composite materials, to avoid side reactions, improve mechanical properties, reduce reaction costs and time costs

Active Publication Date: 2022-01-21
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, since melamine cyanurate is a planar network composed of multiple hydrogen bonds, it is easy to form hydrogen bond crosslinking. It is used as a flame retardant alone in epoxy resin, and it is easy to agglomerate when mixed with epoxy resin. Can affect the compatibility with matrix epoxy resin, in the prior art at present, melamine cyanurate is mainly applied in the resin material by the mode of coating and compounding, for example the patent document that application publication number is CN109705403B (compared with Document 1) discloses a melamine cyanurate microencapsulated red phosphorus flame retardant and a preparation method thereof. The microencapsulated red phosphorus product coated with melamine cyanurate is obtained by coating, which overcomes the red phosphorus flame retardant. The application defect of phosphorus as a flame retardant, but the coating method of reference document 1 may lead to the defect technical problem of the decline in the mechanical properties of the composite material; another example is a cobalt phosphate-melamine cyanide disclosed by the patent application publication number CN110982122A Urate-reactive flame retardant and its preparation method and application (reference document 2), through compounding, the zirconium phosphate-melamine cyanurate reactive flame retardant is activated to improve the flame retardant in the Compatibility in polyurethane, however, this compounding method of Reference 2 will also lead to a decrease in the mechanical properties of the composite material, and it has not been proven that it can be effectively used in epoxy resin

Method used

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  • Melamine cyanurate derivative covalent triazine framework flame retardant, preparation method and application thereof
  • Melamine cyanurate derivative covalent triazine framework flame retardant, preparation method and application thereof
  • Melamine cyanurate derivative covalent triazine framework flame retardant, preparation method and application thereof

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Effect test

Embodiment 1

[0045] The preparation of melamine cyanurate derivative covalent triazine frame flame retardant specifically comprises the following steps:

[0046]Disperse 20.4g of melamine cyanurate into a three-necked flask filled with 100mL of tetrahydrofuran, place it in a water bath filled with ice cubes and stir, and control the temperature at 0-5°C. Then dissolve 5.7mL of phenylphosphoryl dichloride in 50mL of tetrahydrofuran, stir with a glass rod for 3-5min, and slowly drop the solution into the three-necked flask with a rubber dropper after dissolving. Ten minutes after the dropwise addition, 10 mL of triethylamine was added. After the addition of triethylamine, it was stirred at 0-5° C. for 6 h, and then the temperature was raised to 25° C. and stirred for 4 h.

[0047] Vacuum filter the mixed liquid after the reaction to obtain a precipitate, then fully wash with tetrahydrofuran, ethanol and deionized water to remove residual triethylamine, triethylamine hydrochloride and other i...

Embodiment 2

[0050] The preparation of the melamine cyanurate derivative covalent triazine frame flame-retardant epoxy resin composite material specifically comprises the following steps:

[0051] Preheat the epoxy resin in a blast oven for 15 minutes at a temperature of 85°C, then weigh 79.2g of epoxy resin and add them to 1g of melamine cyanurate derivative covalent triazine framework, and set the temperature at 80°C After stirring for 10 minutes under heating in a water bath, add 19.8g of 4,4-diaminodiphenylmethane respectively, and continue stirring for 10 minutes. After the stirring is completed, vacuumize to remove air bubbles, and then pour the mixture into a standard-sized polytetrafluoroethylene mold coated with silicone oil. , after being put into an oven for solidification, cooling and demoulding, and Example 2 was obtained. For comparison, pure epoxy resins were prepared. Add 25g of 4,4-diaminodiphenylmethane to 100g of epoxy resin, stir in a water bath at 80°C for 10min, then...

Embodiment 3

[0055] The preparation of the melamine cyanurate derivative covalent triazine frame flame-retardant epoxy resin composite material specifically comprises the following steps:

[0056] Place the epoxy resin in a blast oven for preheating for 15 minutes, and the oven temperature is 85°C, then weigh 76g of epoxy resin and add them to 5g of melamine cyanurate derivative covalent triazine frame flame retardant respectively. After heating and stirring in a water bath at 80°C for 10 minutes, add 19g of 4,4-diaminodiphenylmethane respectively, and continue stirring for 10 minutes. After the stirring is completed, vacuumize to remove air bubbles, and then pour the mixture into a standard-sized polytetrafluoroethylene mold coated with silicone oil. After being put into an oven for solidification, cooling and demoulding obtained Example 3, wherein the UL-94 test sample size was 130×13×3mm 3 .

[0057] The present invention only needs 5wt% melamine cyanurate derivatives covalent triazine...

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Abstract

The invention belongs to the technical field of flame-retardant macromolecules, and particularly discloses a melamine cyanurate derivative covalent triazine framework flame retardant, a preparation method and application thereof. The preparation method comprises the steps that firstly, phosphorus-chlorine groups of phenyl phosphoryl dichloride react with amine in melamine cyanurate, so that hydrogen bonds in the melamine cyanurate are reduced, and the purpose of reducing the group polarity is reached, then on the basis, the preparation method of the melamine cyanurate derivative covalent triazine framework flame retardant is developed, and the melamine cyanurate derivative covalent triazine framework flame retardant is applied to flame-retardant epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of flame retardant polymers, and in particular relates to a melamine cyanurate derivative covalent triazine frame flame retardant and its preparation method and application. Background technique [0002] As one of the most important thermosetting resins, epoxy resin has been widely used in coatings, Adhesives, sealing materials and electronic components. However, like most organic polymer materials, epoxy resin is flammable, which greatly limits the application range of epoxy resin. Therefore, improving the flame retardant performance of epoxy resin has important practical significance for broadening the application of epoxy resin. [0003] For a long time, traditional halogen-containing flame retardants have been considered as an effective method to improve the flame retardancy of epoxy resins due to their low cost and high flame retardant efficiency, but they are prone to produce toxic and corrosive fume...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/02C08L63/00C08L85/02
CPCC08G79/02C08L63/00C08L2201/02C08L85/02
Inventor 喻源储艳鹏陈忠伟
Owner NANJING TECH UNIV
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