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Phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure and synthesis method of intumescent flame retardant

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 the problems of insufficient proportion, char formation performance and flame retardancy performance, etc., and achieve reasonable proportion and good char formation Ability to promote the effect of charring

Active Publication Date: 2017-12-01
SHUNDE POLYTECHNIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In these patents and synthesis methods, the ratio of acid source-carbon source and gas source is not suitable to varying degrees, and the char-forming performance and flame-retardant performance need to be continuously improved. Therefore, it is necessary to develop flame retardants with better performance.

Method used

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  • Phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure and synthesis method of intumescent flame retardant
  • Phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure and synthesis method of intumescent flame retardant
  • Phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure and synthesis method of intumescent flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The synthesis steps of phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure are as follows:

[0033] step one

[0034] Add 250mL of acetonitrile to 1000mL, cool to -10℃, add 153.33g (1mol) of phosphorus oxychloride (POCl 3 ) Stir and disperse, gradually add 180g (ie 1mol) of 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane (PEPA) and 101.20g ( 1mol) of triethylamine, reacted for 4 hours to obtain the mono-substituted PEPA (POCl 2 -PEPA);

[0035] Step two

[0036] In another container, add 120.20g (2mol) of ethylenediamine, 50mL of acetonitrile and 202.40g (2mol) of triethylamine and mix, cool to -10°C, slowly add 296.83g (1mol) of PEPA-containing One yuan substitution (POCl 2 -PEPA), react for 6 hours, and separate the phosphorus-containing diamine intermediate;

[0037] Step three

[0038] Add 184.5g (1mol) of cyanuric chloride into a 1000mL three-necked flask equipped with reflux condenser, stirrer, and constant pres...

Embodiment 2

[0044] The synthesis steps of phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure are as follows:

[0045] step one

[0046] Add 300mL acetonitrile to 1000mL, cool to 10°C, add 153.33g (1mol) phosphorus oxychloride (POCl 3 1) Stir and disperse, gradually add 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane (PEPA) 180g (1mol) and 101.20g triethylamine (1mol) of acetonitrile solution, react for 1 hour to obtain the mono-substituted PEPA (POCl 2 -PEPA);

[0047] Step two

[0048] Add a mixture of 176.30g (2mol) of butanediamine, acetonitrile (50mL) and 202.40g (2mol) of triethylamine in another container, cool to 10°C, and slowly add dropwise the 296.83g (1mol) obtained in step 1 The unary substitution of PEPA (POCl 2 -PEPA), react for 3 hours, and separate the phosphorus-containing diamine intermediate;

[0049] Step three

[0050] Add 184.5g (1mol) of cyanuric chloride into a 1000mL three-necked flask equipped with reflux cond...

Embodiment 3

[0056] The synthesis steps of phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure are as follows:

[0057] step one

[0058] Add 300mL acetonitrile to 1000mL, cool to 0℃, add 153.33g (1mol) of phosphorus oxychloride (POCl 3 ) Stir and disperse, gradually add 180g (1mol) of 1-oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane (PEPA) and 101.20g (1mol). ) Triethylamine, reacted for 2.5 hours to obtain the mono-substituted PEPA (POCl 2 -PEPA);

[0059] Step two

[0060] In another container, add 120.20g (2mol) of ethylenediamine, 50mL of acetonitrile, 202.40g (2mol) of triethylamine and mix them, cool to 0°C, and slowly add dropwise the 296.83g (1mol) obtained in step 1 ) The unary substitution of PEPA (POCl 2 -PEPA), react for 4.5 hours, and separate the phosphorus-containing diamine intermediate;

[0061] Step three

[0062] Add 184.5g (1mol) of cyanuric chloride into a 1000mL three-necked flask equipped with reflux condenser, sti...

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Abstract

The invention relates to a phosphorus-nitrogen-silicon intumescent flame retardant containing a triazine ring and a cage structure and a synthesis method of the intumescent flame retardant. The synthesis method comprises the steps as follows: a solvent is added to a container, phosphorus oxychloride is added and stirred to be dispersed, PEPA (1-oxy phospha-4-(hydroxymethyl)-2,6,7-trioxabicyclo[2.2.2]octane) and an acid-binding agent are dropwise added step by step, and a PEPA-containing unitary substituent is obtained; substances with diamine or dihydric alcohol are added to the other container and mixed with the solvent and the acid-binding agent, the PEPA-containing unitary substituent is slowly dropwise added, and a phosphorous-containing diamine intermediate is obtained after separation; the solvent is added to a container provided with a reflux condenser and the like, cyanuric chloride is added and stirred to be dispersed, an amino silane coupling agent and the acid-binding agent are dropwise added step by step, and a silicon-containing unitary substituent is obtained; the mixture of the phosphorous-containing diamine intermediate and the acid-binding agent is slowly dropwise added, cooling, washing and drying are performed, and a powdery solid, namely, the phosphorus-nitrogen-silicon intumescent flame retardant containing the triazine ring and the cage structure, is obtained. The phosphorus-nitrogen-silicon intumescent flame retardant has the advantages that the flame retardant has certain polymerization degree, high molecular weight, higher charcoal forming amount and better thermal stability, the proportion of acid sources, carbon sources and gas sources in molecular structures is relatively proper and the like.

Description

Technical field [0001] The invention belongs to the technical field of environmentally friendly halogen-free flame retardant products. Specifically, the invention relates to a phosphorus-nitrogen-silicon intumescent flame retardant containing a triazine ring and a cage structure and a synthesis method thereof. Background technique [0002] Polymer materials are widely used, bringing convenience to production and life. However, their flammable characteristics limit their use in occasions with high flame retardant requirements. Therefore, flame retardant modification of polymer materials has become one of the important content of their modification. [0003] Halogen-containing flame retardants, especially bromine-containing flame retardants, have excellent flame retardant properties, but when such flame retardants burn, they generate a large amount of dense smoke and corrosive gases, which causes great environmental pollution. Based on environmental considerations, it is particularl...

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 SHUNDE POLYTECHNIC
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