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Thiotriazinone 'phosphorus-silicon-nitrogen' oligomer-form intumescent flame retardant and synthetic process thereof

A technology of intumescent flame retardant and synthesis method, which is applied in the field of environmentally friendly halogen-free flame retardant products, can solve problems such as insufficient proportions, and achieve the effects of reasonable proportions, good char formation ability, and good char formation properties

Active Publication Date: 2017-10-24
广州光通科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is not suitable for use as an additive flame retardant in plastics, coatings, etc.
[0009] These patents and synthesis methods have the following problems to varying degrees: the ratio of acid source-carbon source and gas source is not suitable enough, and the char-forming performance and flame-retardant performance need to be further improved

Method used

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  • Thiotriazinone 'phosphorus-silicon-nitrogen' oligomer-form intumescent flame retardant and synthetic process thereof
  • Thiotriazinone 'phosphorus-silicon-nitrogen' oligomer-form intumescent flame retardant and synthetic process thereof
  • Thiotriazinone 'phosphorus-silicon-nitrogen' oligomer-form intumescent flame retardant and synthetic process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The synthesis steps of the "phosphorus-silicon-nitrogen" oligomer type intumescent flame retardant containing a triazine ring are as follows:

[0038] step one

[0039] In a 1000ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 92.25g (ie 0.5mol) of cyanuric chloride, then add 200ml of acetonitrile, and place the three-necked flask in an oil bath. Stir well to disperse cyanuric chloride evenly, add 110.69 g (0.5 mol) of γ-aminopropyltriethoxysilane (KH550) dropwise into the three-necked bottle, and 50.6 g (0.5 mol) of triethyl The amine is added dropwise with a constant pressure funnel, the pH is controlled between 5-7, the reaction temperature is controlled at -10°C, and the reaction time is 4 hours to obtain a silicon-containing monobasic substituted product of cyanuric chloride (CNC-Si);

[0040] step two

[0041] Add 60.10g (ie 1mol) of ethylenediamine, 350mL of chloroform and 101.19g (ie 1mol) of triet...

Embodiment 2

[0049] The synthesis steps of the "phosphorus-silicon-nitrogen" oligomer type intumescent flame retardant containing a triazine ring are as follows:

[0050] step one

[0051] In a 1000ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 184.5g (ie 1mol) of cyanuric chloride, then add 400ml of acetone, place the three-necked flask in an oil bath, and fully Stir to disperse cyanuric chloride evenly, add 179.30 g (1mol) of γ-aminopropyltrimethoxysilane (KH551) dropwise into the three-necked flask, and 101.20 g (1mol) of triethylamine with a constant pressure funnel Add dropwise, control the pH between 5-7, control the reaction temperature at 0°C, and the reaction time is 2.5 hours to obtain a silicon-containing monosubstituted cyanuric chloride (CNC-Si);

[0052] step two

[0053] Add 120.20 g (2mol) of ethylenediamine, 202.40g (ie 2mol) of triethylamine and (500mL) chloroform into another 1000mL three-necked flask, mi...

Embodiment 3

[0061] The synthesis steps of the "phosphorus-silicon-nitrogen" oligomer type intumescent flame retardant containing a triazine ring are as follows:

[0062] step one

[0063] In a 1000ml three-necked flask equipped with a reflux condenser, a stirrer, and a constant pressure dropping funnel, add 184.5g (ie 1mol) of cyanuric chloride, then add 400ml of acetone, place the three-necked flask in an oil bath, and fully Stir to disperse cyanuric chloride evenly, add 191.34 g (ie 1 mol) of γ-aminopropylmethyldiethoxysilane (KH552) dropwise into the three-necked bottle, and 60.59 g (ie 0.5 mol) of triethylene Diamine is added dropwise with a constant pressure funnel, the pH is controlled between 5-7, the reaction temperature is controlled at 10°C, and the reaction time is 1 hour to obtain a silicon-containing monobasic substituted product (CNC-Si) of cyanuric chloride.

[0064] step two

[0065] Add 120.20 g (ie 2 mol) of ethylenediamine, 121.18 g (2 mol) of triethylenediamine and 5...

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PUM

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Abstract

The invention relates to a thiotriazinone 'phosphorus-silicon-nitrogen' oligomer-form intumescent flame retardant and a synthetic process thereof. The synthetic process is characterized by including the steps of adding a solvent into a container that is fitted with a reflow condenser, a stirrer and a constant-pressure dropper, adding cyanuric chloride, stirring and dispersing, dropwise adding an aminosilane coupling agent and an acid-binding agent to obtain a silicon-bearing unitary substituent; adding a diamine or diol substance into another container, mixing with a solvent and an acid-binding agent, dropwise adding a phosphorus-bearing compound slowly, and separating to obtain a phosphorus-bearing intermediate; dropwise adding the phosphorus-bearing intermediate of step II into a container with the silicon-bearing unitary compound, and dropwise adding an acid-binding agent to obtain a phosphorus-bearing silicon dimer; dropwise adding the phosphorus-bearing silicon dimer, the phosphorus-bearing diamine intermediate, and an acid-binding agent into a reaction container that contains a solvent. The retardant of the invention has the advantages, for instance, the retardant has good char-forming capacity, the retardant can form a greater char layer after combustion, intramolecular flame-retarding synergy is given to play, and the yield reaches 91% and above.

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 "phosphorus-silicon-nitrogen" oligomer expansion flame retardant containing a triazine ring and a synthesis method thereof. Background technique [0002] Polymer materials are widely used, bringing great convenience to people's production and life. However, most polymer materials are flammable, which to a certain extent limits their use in occasions with flame-retardant requirements. Therefore, the flame-retardant modification of polymer materials has become one of the focuses of its development. [0003] Based on environmental considerations, halogen-containing flame retardants are gradually restricted. Therefore, the development of halogen-free flame retardants has become an important direction for the development of flame retardants. Intumescent flame retardant (IFR) can form a dense charcoal layer whe...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08L79/04
CPCC08G73/0638C08G73/065C08L79/04C08L2201/02C08L2201/08
Inventor 冯才敏黄健光梁敏仪姜佳丽张浥琨刘洪波
Owner 广州光通科技有限公司
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