Preparation method for nitrogen-containing silica sol synergistic phosphorus flame-retardant epoxy acrylate coating layer

A technology of epoxy acrylate and methacrylic acid, which is applied in the field of flame retardant materials, and can solve the problems of large amount of addition, low burning rate, and easy formation of ammonia water, etc.

Active Publication Date: 2018-07-27
PUTIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogenated flame retardants, although their flame retardant effect is remarkable, the dosage is small, and the cost is low, but halogen-containing flame retardants will produce a large amount of toxic gases at high temperatures, which not only damages the environment, but also poses a threat to human safety
Phosphorus-based flame retardants do not produce toxic gases, and phosphorus elements have a good synergistic effect with nitrogen and silicon elements. The compounded phosphorus-nitrogen and nitrogen-silicon flame retardant EA has the characteristics of low smoke and non-toxicity, but adding Type phosphorus-containing flame retardants usually need to be added in large amounts (20%-40%)
Nitrogen-based flame retardants release a large amount of non-combustible gases at high temperatures, such as carbon dioxi...

Method used

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  • Preparation method for nitrogen-containing silica sol synergistic phosphorus flame-retardant epoxy acrylate coating layer
  • Preparation method for nitrogen-containing silica sol synergistic phosphorus flame-retardant epoxy acrylate coating layer
  • Preparation method for nitrogen-containing silica sol synergistic phosphorus flame-retardant epoxy acrylate coating layer

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preparation example Construction

[0027] A method for preparing a nitrogen-containing silicon sol synergistic phosphorus flame-retardant epoxy acrylate coating, comprising the following steps:

[0028] 1) Preparation of nitrogen-containing silica sol

[0029] Add silane coupling agent KH-570, silane coupling agent KH-550 and distilled water into the beaker, place in a magnetic oil bath and stir, the silane coupling agent KH-570, silane coupling agent KH-550 and distilled water The molar ratio is 0.13-0.17: 0..8-1.2: 0.1 (preferably 0.15: 0.1: 0.1), then slowly add dilute hydrochloric acid with a concentration of 0.8-1.2mol / L until the pH of the solution is 1-2 , then heated to 45-55°C, reacted for 2.5-3.5h, and dried the product in a vacuum oven at 28-35°C for 2.5-3.5h to obtain a colorless transparent viscous solution, namely nitrogen-containing silica sol; the reaction formula is as follows :

[0030]

[0031] Synthetic reaction formula of formula 1 nitrogen-containing silica sol

[0032] 2) Preparatio...

Embodiment 1

[0040] Preparation of nitrogen-containing silica sol

[0041]Add 0.15mol of KH-570 and 0.10mol of KH-550 silane coupling agent and 0.10mol of distilled water into a 250mL beaker, place in a magnetic oil bath and stir, slowly add dilute hydrochloric acid with a concentration of 1mol / L dropwise until The pH value of the solution is between 1-2. Heat to 50°C, react at this temperature for 3 hours, and place in a vacuum oven at 30°C to dry for 3 hours after the reaction is completed, to obtain a colorless transparent viscous solution, ie nitrogen-containing silica sol.

Embodiment 2

[0043] Preparation of TGMAP

[0044] Take 0.1 mol of phosphoric acid in a 500 mL round bottom flask, place it in an ice-water bath and stir, add 0.3 mol of glycidyl methacrylate (GMA) dissolved in 100 mL of acetone dropwise, and then add 0.13 g of phenol. The above-mentioned flask was transferred to an oil bath and heated to 80°C, reacted for 8 hours, then cooled to 60°C, and distilled under reduced pressure for 3 hours to obtain the colorless product TGMAP.

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Abstract

The invention discloses a preparation method for a nitrogen-containing silica sol synergistic phosphorus flame-retardant epoxy acrylate coating layer. The method uses glycidyl methacrylate, phosphoricacid, KH-570 and KH-550 as raw materials to prepare a phosphorus-containing substance TGMAP and a nitrogen-containing silica sol; and the phosphorus-containing substance TGMAP, the nitrogen-containing silica sol and epoxy acrylate are mixed, ultraviolet light curing is performed, and therefore the epoxy acrylate coating layer containing P-N-Si is prepared. The structure, thermal stability and flame retardance of the composite EA coating layer provided by the invention are characterized by an infrared spectrometer, a limiting oxygen index meter and a vertical burning tester, and results show that in the epoxy acrylate coating layer prepared by the method provided by the invention, the nitrogen-containing silica sol is not changed, and as the TGMAP increases, a carbon residual rate and an expansion multiple are increased significantly, after flame time becomes shorter obviously, and an LOI value is increased obviously; and the results indicate that the N-containing silica sol and the TGMAP have a good synergistic flame-retardant effect.

Description

technical field [0001] The invention relates to the technical field of flame retardant materials, in particular to a method for preparing a nitrogen-containing silicon sol in conjunction with a phosphorus flame retardant epoxy acrylate coating. Background technique [0002] Flame-retardant coatings can be applied to the surface of materials that are relatively easy to burn, such as wood, plastics, and cables. It can not only retain the properties of the material itself, but also provide fire protection for the material. The flame retardant mechanism of flame retardant coatings is generally divided into the following categories: (1) Endothermic effect: when an object is burned, a flame retardant with a high ignition point will undergo endothermic decomposition reactions such as dehydration, phase change, or dehalogenated oxygen during the combustion process. , causing the heat on the surface of the coating and the heat in the flame area to be absorbed, thus reducing the rate ...

Claims

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Application Information

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IPC IPC(8): C09D163/10C09D5/18
CPCC08L2201/02C09D5/18C09D163/10C08L83/08
Inventor 郑炳云杨磊
Owner PUTIAN UNIV
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