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Reactive phosphorus-containing halogen-free intumescent flame retardant and synthetic method thereof

A technology of intumescent flame retardant and synthesis method, which is applied in the field of organic flame retardants, can solve the problems that the flame retardant performance of water-based polyurethane cannot meet the requirements, and achieve the effects of great application potential, good compatibility, and high yield

Inactive Publication Date: 2016-02-03
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because its molecule itself does not contain carbon-forming components, its flame retardant performance in waterborne polyurethane cannot meet the requirements.

Method used

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  • Reactive phosphorus-containing halogen-free intumescent flame retardant and synthetic method thereof
  • Reactive phosphorus-containing halogen-free intumescent flame retardant and synthetic method thereof
  • Reactive phosphorus-containing halogen-free intumescent flame retardant and synthetic method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] A reactive phosphorus-containing halogen-free intumescent flame retardant, named: 2,4,8,10-tetraoxa-3,9-diphosphaspiro-3,9-dioxa-3,9-di (3-aminophenyl); English abbreviation: BPPA; molecular formula is C 17 h 20 N 2 o 6 P 2 , the structural formula is:

[0023]

[0024] A reactive phosphorus-containing halogen-free expansion flame retardant, the specific steps are as follows:

[0025] Step 1: Synthesis of BPPB.

[0026] Under the protection of an inert gas, mix 34g (0.25mol) of PER, 300mL of dichloromethane (dried over molecular sieves for 48h), and 79.1g (1mol) of pyridine under an ice bath, stir vigorously for 30min, and then add dropwise 97.5g (0.5 mol) of phenylphosphoryl dichloride in dichloromethane (50 mL), the dropwise addition was completed within 2 hours. The reaction was continued for 0.5 h under ice bath, and then the temperature was raised to 50° C. for reflux reaction for 8 h. Cool to heat up, let stand for 1 day, filter with suction, wash 5-6 t...

Embodiment 2

[0033] A reactive phosphorus-containing halogen-free intumescent flame retardant, named: 2,4,8,10-tetraoxa-3,9-diphosphaspiro-3,9-dioxa-3,9-di (3-aminophenyl); English abbreviation: BPPA; molecular formula is C 17 h 20 N 2 o 6 P 2 , the structural formula is:

[0034]

[0035] A reactive phosphorus-containing halogen-free expansion flame retardant, the specific steps are as follows:

[0036] Step 1: Synthesis of BPPB base.

[0037] Under the protection of an inert gas, 68g (0.5mol) of PER, 600mL of chloroform (dried by molecular sieves for 48h), and 202.4g (2mol) of triethylamine were fully mixed under an ice bath, vigorously stirred for 30min, and then 195.0 g (1mol) of phenylphosphoryl dichloride in chloroform (100mL) was added dropwise within 2h. The reaction was continued for 0.5 h under ice bath, and then the temperature was raised to 60° C. for 5 h under reflux. Cool to room temperature, let stand for 1 day, filter with suction, wash with plenty of water for s...

Embodiment 3

[0043] A reactive phosphorus-containing halogen-free intumescent flame retardant, named: 2,4,8,10-tetraoxa-3,9-diphosphaspiro-3,9-dioxa-3,9-di (3-aminophenyl); English abbreviation: BPPA; molecular formula is C 17 h 20 N 2 o 6 P 2 , the structural formula is:

[0044]

[0045] A reactive phosphorus-containing halogen-free expansion flame retardant, the specific steps are as follows:

[0046] Step 1: Synthesis of BPPB.

[0047] N 2 Under protection, add 17g (0.125mol) of PER, 150mL of chloroform (dried on molecular sieves for 48h), 60.6g (0.5mol) of N,N-dimethylaniline into a 250mL three-necked flask under ice bath, and stir vigorously for 30min , and then 48.8 g (0.25 mol) of phenylphosphoryl dichloride in chloroform (25 mL) was added dropwise to the system, and the dropwise addition was completed within 2 hours. The reaction was continued for 0.5 h under ice bath, and then the temperature was raised to 50° C. for 6 h under reflux. Cool to heat up, let stand for 1 ...

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Abstract

The invention relates to a reactive phosphorus-containing halogen-free intumescent flame retardant and a synthetic method thereof, belonging to the field of organic fire retardants. The reactive phosphorus-containing halogen-free intumescent flame retardant has a structural formula as described in the specification. The synthetic method comprises the following steps: preparing an intermediate 2,4,8,10-tetraoxa-3,9-diphosphaspirocyclo-3,9-dioxy-3,9-diphenyl (BPPB) from primary raw materials consisting of pentaerythritol and dichlorophenylphosphine oxide; then preparing a phosphorus-containing compound containing two nitro groups, i.e., 2,4,8,10-tetraoxa-3,9-diphosphaspirocyclo-3,9-dioxy-3,9-di(3-nitrophenyl) (BPPN), by using fuming nitric acid reduction method; and reducing BPPN into the final product 2,4,8,10-tetraoxa-3,9-diphosphaspirocyclo-3,9-dioxy-3,9-di(3-aminophenyl) (BPPA) by using a reduction method. The method is simple to operate and has a good industrial application value. The prepared intumescent flame retardant has excellent flame retardation performance and good heat stability.

Description

technical field [0001] The invention relates to a reactive phosphorus-containing halogen-free expansion flame retardant and a synthesis method thereof, belonging to the field of organic flame retardants. Background technique [0002] Reactive flame retardant polymer materials refer to the introduction of flame retardants into the molecular structure of polymer materials as reactants, so that they have flame retardancy without adding flame retardants, and can achieve a certain degree of flame retardancy. level. The reactive flame retardant polymer material is a modification of the polymer material at the molecular level, which fundamentally overcomes the related interface problems, and directly introduces flame retardant elements or structures into the molecules of the polymer material so that the amount of modifier It is greatly reduced, and the negative impact on material performance is also greatly reduced. There is no problem of volatile, leaching, migration and exudatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5317C08L75/04C08L63/00
Inventor 柴春鹏罗运军吴刚林嘉伦葛震
Owner BEIJING INSTITUTE OF TECHNOLOGYGY