Trine expansion type flame retardant and synthetic method thereof

An intumescent flame retardant, a trinity technology, applied in the field of "trinity" intumescent flame retardant and its synthesis, can solve the problems of high moisture absorption, insufficient proportion, and many hydroxyl groups in the flame retardant, and achieve good results. Excellent charcoal properties, thermal stability, and flame retardancy

Active Publication Date: 2017-09-01
蕉岭金鹏精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Patent CN105968410A is an intumescent flame retardant containing polyhydroxyl and phosphorus-based triazine rings, which has a good flame-retardant effect on polypropylene, but the flame retardant contains many hydroxyl groups and has high moisture absorption, which will affect the subsequent use of composite materials. have a certain i

Method used

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  • Trine expansion type flame retardant and synthetic method thereof
  • Trine expansion type flame retardant and synthetic method thereof
  • Trine expansion type flame retardant and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0036] Embodiment one

[0037] step one

[0038] In a 1000ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 92.25g (0.5mol) of cyanuric chloride, then add 200ml of acetonitrile, place the three-necked flask in an oil bath, and fully Stir to disperse cyanuric chloride evenly, and drop 90.0g (ie 0.5mol) of 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2. 2] Octane (PEPA), 50.6g (0.5mol) of triethylamine was added dropwise with a constant pressure funnel, the pH was controlled between 5-7, the reaction temperature was controlled at 35°C, and the reaction time was 3 hours to obtain three A monobasic substitute for polycyanogen chloride (CNC-PEPA).

[0039] step two

[0040] Add a mixture of ethylenediamine 60.10 g (1mol), chloroform (350mL) and triethylamine 101.19g (1mol) into another 1000mL three-neck flask, cool to 0°C in an ice bath or freezing reactor, and slowly 97.49 g (0.5 mol) of phenylphosphoryl dichl...

Example Embodiment

[0043] Embodiment two

[0044] step one

[0045] In a 500ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 46.13g (0.25mol) of cyanuric chloride, then add 200ml of acetone, place the three-necked flask in an oil bath, and fully Stir to disperse cyanuric chloride evenly, add 45.0g (0.25mol) of PEPA dropwise to the three-necked bottle, add 25.3g (0.25mol) of triethylamine dropwise with a constant pressure funnel, and control the pH between 5-7 During this period, the reaction temperature was controlled at 30°C and the reaction time was 3 hours to obtain the monosubstituted cyanuric chloride (CNC-PEPA).

[0046] step two

[0047] Add 30.05g (0.5mol) of ethylenediamine and 50.60g (0.5mol) of triethylamine mixture and solvent dioxane (250mL) into another 500mL three-neck flask, and cool to 10°C in a refrigerated reactor. Slowly add 62.5 g (0.25 mol) of anilinophosphoryl dichloride dropwise and react for 4 hours to obt...

Example Embodiment

[0050] Embodiment Three

[0051] step one

[0052] In a 1000ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 184.5g (1mol) of cyanuric chloride, then add 500ml of acetone, place the three-necked flask in an oil bath, and stir thoroughly , to make the cyanuric chloride disperse evenly, add 180.0g (1mol) PEPA dropwise to the there-necked bottle, add 101.19g (1mol) triethylamine dropwise with a constant pressure funnel, control the pH between 5-7, and the reaction temperature The temperature is controlled at 30°C, and the reaction time is 3 hours to obtain the monobasic substituted product of cyanuric chloride (CNC-PEPA).

[0053] step two

[0054] Add 124.18 g (2mol) of ethylene glycol, chloroform (400mL) and 202.38g (2mol) of triethylamine mixture into a 1000mL three-necked flask, cool to -10°C in an ice-bath reactor, and slowly add 211.0 g (1mol) of phenoxyphosphoryl dichloride was reacted for 5 hours to obtain ...

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PUM

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Abstract

The invention relates to a trine expansion type flame retardant and a synthetic method thereof. The synthetic method is characterized by comprising the following steps: adding a solvent into a container, adding cyanuric chloride and 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2] octane into the container, cooling to 0-45 DEG C in water bath or oil bath and stirring and dispersing, dropwise adding an acid-binding agent to react step by step, thereby obtaining unary substitute; adding matters containing aliphatic diamine or aliphatic dihydric alcohol and a mixture of the solvent and the acid-binding agent into another container, cooling to -10 to 10 DEG C in ice bath or a freezing reactor, slowly dropwise adding a phosphorus-containing compound to react, thereby obtaining phosphorus-containing intermediate; adding the obtained unary substitute (CNC-PEPA) and the obtained phosphorus-containing intermediate into a reaction container with the solvent, dropwise adding the acid-binding agent, heating to 80-130 DEG C to react, cooling, washing and drying to obtain powder solid, namely the trine expansion type flame retardant. The trine expansion type flame retardant has the advantages of being great in molecular weight, relatively moderate in proportion of an acid source, a carbon source and a gas source in a molecular structure, relatively high in char forming content, relatively good in thermal stability and the like.

Description

technical field [0001] The invention belongs to the technical field of environment-friendly halogen-free flame retardant products. Specifically, the invention relates to a "trinity" intumescent flame retardant containing caged phosphate, a triazine structure and a benzene ring structure and a synthesis method thereof. Background technique [0002] Polymer materials are widely used in people's production and life, which brings great convenience. However, since most polymer materials are flammable materials, their use in places with flame retardant requirements is greatly limited. Therefore, flame retardant modification has become one of the important contents of polymer material modification. [0003] Halogen-containing flame retardants, especially bromine-containing flame retardants, when compounded with antimony trioxide, have a good flame-retardant effect on polymer materials. However, this type of flame retardant will release a large amount of toxic and harmful substance...

Claims

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Application Information

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IPC IPC(8): C08G73/06
CPCC08G73/065
Inventor 冯才敏黄健光梁敏仪张浥琨刘洪波
Owner 蕉岭金鹏精细化工有限公司
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