A kind of intumescent flame retardant and preparation method thereof

An intumescent flame retardant and solvent technology, applied in the directions of adhesives, adhesive types, adhesive additives, etc., can solve problems such as poor thermal stability, and achieve the effects of simple operation, wide applicability of the preparation process, and broad application prospects.

Active Publication Date: 2021-03-16
浙江拓锐新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a novel intumescent flame retardant and its preparation method in order to overcome the disadvantage of poor thermal stability of the intumescent flame retardant in the prior art. The intumescent flame retardant has excellent Thermal stability and excellent flame retardancy (UL-94 flame retardant grade can reach V-1 grade), in addition, it also has low smoke density

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Preparation of Mannich base

[0027] (1) At 60°C, add 30g of paraformaldehyde and 105g of diethanolamine into the reaction kettle to react for 2 hours to obtain the 3-hydroxyethyl-1,3-oxazolidine reaction solution, which is distilled under reduced pressure at 125-130°C / 8000Pa The product 3-hydroxyethyl-1,3-oxazolidine was obtained;

[0028] (2) At 70°C, add 47g of resorcinol and 117g of 3-hydroxyethyl-1,3-oxazolidine obtained in step (1) into the reactor for 3 hours to obtain Mannich alkali.

[0029] 2. Preparation of intumescent flame retardant

[0030] (1) Under a helium atmosphere, add 10 g of melamine, 25 g of Mannich base, 18 g of phosphorus oxychloride and 200 g of toluene into a reaction kettle, heat to a constant temperature of 50° C. and react for 1 h;

[0031] (2) Heat and reflux until the hydrogen chloride gas is completely volatilized, and cool to 10° C. to obtain the intumescent flame retardant.

Embodiment 2

[0037] 1. Preparation of Mannich base

[0038] (1) At 60°C, add 30g of paraformaldehyde and 105g of diethanolamine into the reaction kettle to react for 2 hours to obtain the 3-hydroxyethyl-1,3-oxazolidine reaction solution, which is distilled under reduced pressure at 125-130°C / 8000Pa The product 3-hydroxyethyl-1,3-oxazolidine was obtained;

[0039] (2) At 70°C, add 47g of resorcinol and 117g of 3-hydroxyethyl-1,3-oxazolidine obtained in step (1) into the reactor for 3 hours to obtain Mannich alkali.

[0040] 2. Preparation of intumescent flame retardant

[0041] (1) Under a helium atmosphere, add 10 g of melamine, 25 g of Mannich base, 18 g of phosphorus oxychloride and 200 g of toluene into a reaction kettle, heat to a constant temperature of 50° C. and react for 1 h;

[0042] (2) Heat and reflux until the hydrogen chloride gas is completely volatilized, and cool to 10-30° C. to obtain the intumescent flame retardant.

Embodiment 3

[0044] 1. Preparation of Mannich base

[0045] (1) At 80°C, react 83g of formaldehyde aqueous solution (37%) with 105 diethanolamine for 4 hours to obtain a 3-hydroxyethyl-1,3-oxazolidine reaction solution, which is then distilled under reduced pressure at 125-130°C / 8000Pa to obtain Product 3-hydroxyethyl-1,3-oxazolidine;

[0046] (2) At 70-90°C, add 47g of hydroquinone or 117g of 3-hydroxyethyl-1,3-oxazolidine obtained in step (1) into the reaction kettle for 3-5h to obtain Mannich alkali.

[0047] 2. Preparation of intumescent flame retardant

[0048] (1) Under a helium atmosphere, add 10 g of melamine, 25 g of Mannich base, 18 g of phosphorus oxychloride and 200 g of toluene into a reaction kettle, heat to a constant temperature of 50° C. and react for 1 h;

[0049] (2) Heat and reflux until the hydrogen chloride gas is completely volatilized, and cool to 10° C. to obtain the intumescent flame retardant.

[0050] 2. Preparation of intumescent flame retardant

[0051] (...

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PUM

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Abstract

The invention discloses an intumescent flame retardant and a preparation method thereof. The intumescent flame retardant is prepared from, by weight, 10 parts of melamine, 25-60 parts of Mannich base,18-36 parts of a phosphorus-containing compound and 200-250 parts of a solvent. Polyurethane prepared by the intumescent flame retardant has the excellent thermal stability, low smoke density and a good flame retardant property; the raw material components of the intumescent flame retardant can be free of halogen-based flame retardants, a large amount of toxic and corrosive hydrogen halide cannotbe released during combustion, the environment is protected, the raw materials have abundant sources and low cost, the preparation process is high in applicability and easy to operate, and thereforethe intumescent flame retardant has broad application prospects.

Description

technical field [0001] The invention relates to an intumescent flame retardant and a preparation method thereof. Background technique [0002] The development of science and technology and the enhancement of people's safety and environmental awareness have put forward higher and more requirements for the flame retardancy and environmental protection of materials. Adding flame retardants is an effective method to improve the flame retardancy of materials. In addition to flame retardant properties, flame retardants should also be environmentally friendly. [0003] Intumescent flame retardants, as a new type of environmentally friendly flame retardants, have received widespread attention in the field of flame retardants in the world in recent years. It has a unique flame retardant mechanism, does not produce toxic gases, and produces low smoke. In line with today's requirements for protecting the ecological environment, it opens up a halogen-free path for the development of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/3492C08K5/521C08K5/523C09J11/06C09J175/08
CPCC08K5/34928C08K5/521C08K5/523C09J11/06C09J175/08
Inventor 张志勇傅晓文赵一朵
Owner 浙江拓锐新材料科技有限公司
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