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Triazine charring agent, preparation method therefor and application thereof

A technology of triazines and char-forming agents, which is applied in the field of materials, can solve the problems of low thermal stability of products, large amount of organic solvents, and difficult follow-up treatment, etc., achieve good char-forming and flame-retardant effects, short reaction cycle, Good charcoal and flame retardant effect

Active Publication Date: 2016-03-23
山东艾孚特科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, patents on the preparation of some triazine derivatives and their application as charring agents or flame retardants have been continuously disclosed (CN1314898A, CN101586033A, CN101007953, CN201010165863.6, CN200710071927.4, WO9744377, JP0583065A1, ZL2005100102043.4, 42) These patents basically have the disadvantages of large amount of organic solvent (the organic solvent is mainly acetone), serious environmental pollution, or difficult follow-up treatment, low thermal stability of the product, low carbon residue, etc., and the reaction cycle is generally too long. above

Method used

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  • Triazine charring agent, preparation method therefor and application thereof
  • Triazine charring agent, preparation method therefor and application thereof
  • Triazine charring agent, preparation method therefor and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Take a 2L four-neck round-bottomed flask with a stirrer, thermometer, condenser and constant pressure dropping funnel, add 132g of hypophosphorous acid aqueous solution (50% content), 210.6g diethanolamine (99.7% content), and 1056g water into the flask , start stirring, add 17g of hydrochloric acid (content 31%), then raise the temperature to 95-100°C, add 170.3g of formaldehyde aqueous solution (content 37%) dropwise for 0.5-1h, continue the reaction for 3 hours after the addition, add 126g of melamine to continue the reaction After 2 hours, cool down, filter, and dry to obtain 412.1 g of charcoal agent, with a yield of 96.7% based on hypophosphorous acid.

[0036] figure 1 It is the infrared spectrogram of the obtained char-forming agent. It can be seen from the figure that there are melamine groups, diethanolamine groups and phosphorus-oxygen groups, which are consistent with the structure of the new synthesized char-forming agent.

Embodiment 2

[0038] Take a 2L four-neck round bottom flask equipped with a stirrer, thermometer, condenser and constant pressure dropping funnel, add 132g of hypophosphorous acid aqueous solution (50% content), 210.6g of diethanolamine, and 1320g of water into the flask, and start stirring , add 17g of hydrochloric acid (content 31%), then raise the temperature to 95-100°C, add 170.3g of formaldehyde aqueous solution (content 37%) dropwise for 0.5-1h, continue the reaction for 3h after the dropwise addition, add 126g of melamine, continue the reaction for 2h, then cool down, Filtration and drying yielded 418.1 g of a novel char-forming agent, with a yield of 98.1% based on hypophosphorous acid.

Embodiment 3

[0040] Take a 2L four-neck round bottom flask equipped with a stirrer, thermometer, condenser and constant pressure dropping funnel, add 132g of hypophosphorous acid aqueous solution (50% content), 210.6g of diethanolamine, and 1584g of water into the flask, and start stirring , add 17g of hydrochloric acid (content 31%), then raise the temperature to 95-100°C, add 170.3g of formaldehyde aqueous solution (content 37%) dropwise for 0.5-1h, continue the reaction for 3h after the dropwise addition, add 126g of melamine, continue the reaction for 2h, then cool down, Filtration and drying yielded 417.9 g of a novel char-forming agent, with a yield of 98.1% based on hypophosphorous acid.

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Abstract

The present invention discloses a triazine charring agent, a preparation method therefor and application thereof. The preparation method comprises the following steps: performing an Mannich reaction on hypophosphorous acid, diethanol amine, and formaldehyde catalyzed by hydrochloric acid in an aqueous phase; after the reaction, adding melamine to the reaction solution to react sequentially; and obtaining the triazine charring agent with the following structural formula. The present invention also provides application of the charring agent as a raw material of a flame retardant, as well as a preparation method of the flame retardant. According to the method disclosed by the present invention, reaction conditions are mild, a process flow of operations is simple, a reaction period is short, and post treatment is simple. The resulting charring agent has good expansibility, high thermal stability, a large amount of carbon residue, a good charring effect, and good compatibility with a polymer. The charring agent can be made into the flame retardant by mixing with ammonium polyphosphate, polypropylene, and the like, with excellent inflaming retarding performance and little influence on mechanical properties.

Description

technical field [0001] The invention relates to a triazine char forming agent and a preparation method thereof, and also relates to a flame retardant containing the triazine char forming agent and a preparation method of the flame retardant, belonging to the field of material technology. Background technique [0002] Intumescent flame retardant (IFR) is a halogen-free flame retardant with phosphorus and nitrogen as the main components. It is one of the types of green and environmentally friendly flame retardants widely used in recent years, because it not only overcomes It is easy to emit irritating and corrosive gas and smoke, many molten droplets, and easily cause suffocation of personnel. It also overcomes the adverse effects of inorganic flame retardants on material mechanics and processing properties due to large additions. Due to its unique flame retardant mechanism, halogen-free, low smoke, low toxicity, and the generated carbon layer can effectively prevent polymer d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C07D251/54C07D251/56C08L23/12C08K3/32C08K5/5313
CPCY02P20/52C07F9/301C07D251/54C07D251/56C08K3/32C08K5/5313C08K2003/323
Inventor 岳涛邢文国陈琦冯维春周倜张健孟宪兴李培培游淇杨旭
Owner 山东艾孚特科技有限公司
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