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Phosphorus and nitrogen oligomer flame retardant and preparation method thereof

A flame retardant and oligomer technology, applied in the field of phosphorus nitrogen oligomer flame retardant and its preparation, can solve the problems of inability to meet the requirements of processing temperature, large impact on material mechanical properties, poor thermal stability, etc. Commercial value and market prospects, good thermal stability, easy post-processing effects

Pending Publication Date: 2019-12-10
ZHEJIANG FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing phosphorus-nitrogen-based flame retardants have poor thermal stability and are easy to migrate, so that most of the existing phosphorus-nitrogen-based flame retardants have an initial decomposition temperature in the range of 160-210°C
When added to engineering plastics, it has a great impact on the mechanical properties of the material, and cannot meet the requirements of high processing temperature and easy-to-degrade engineering plastics, so it needs to be improved.

Method used

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  • Phosphorus and nitrogen oligomer flame retardant and preparation method thereof
  • Phosphorus and nitrogen oligomer flame retardant and preparation method thereof
  • Phosphorus and nitrogen oligomer flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Mix 0.06 mol piperazine and 0.15 mol triethylamine dissolved in 156 g of acetonitrile, heat to reflux temperature, and add 0.066 mol phenylphosphonic dichloride diluted with solvent drop by drop. After the dropwise addition is completed within 2 hours, the Keep the reaction at the reflux temperature of 60-80°C for 6-8 hours; after the reaction, distill the solvent under reduced pressure, dissolve the residue in ethanol, filter to remove triethylamine hydrochloride, pour the filtrate into a large amount of ether to precipitate a brown precipitate, filter, Washing with water several times, and vacuum-drying at 80° C. to obtain the phosphorus nitrogen oligomer flame retardant phenylphosphonopiperazine, the yield is 50.0%.

[0036] The infrared spectrogram of the prepared phosphorus nitrogen oligomer flame retardant, 1 H NMR and 31 P-NMR see respectively Figure 1-Figure 3 .

[0037] Phenylphosphonopiperazine test analysis results are as follows:

[0038] FTIR (KBr, cm-...

Embodiment 2

[0042] Mix 0.06mol 1,4-butanediamine and 0.15mol triethylamine dissolved in 156g acetonitrile, heat to reflux temperature, add 0.066mol phenylphosphonic acid dichloride diluted with solvent drop by drop, drop within 2h After the addition is complete, keep the reaction at the reflux temperature of 60-80°C for 6-8h; after the reaction, distill the solvent off under reduced pressure, dissolve the residue in ethanol, filter to remove triethylamine hydrochloride, pour the filtrate into a large amount of ether to precipitate The brown precipitate was filtered, washed with water several times, and vacuum-dried at 80° C. to obtain a phosphorus nitrogen oligomer flame retardant phenylphosphonobutylene diamine with a yield of 2.5%.

Embodiment 3

[0044] Mix 0.06mol 1,6-hexanediamine and 0.15mol triethylamine dissolved in 156g acetonitrile, heat to reflux temperature, add 0.066mol phenylphosphonic dichloride diluted with solvent drop by drop, drop within 2h After the addition is complete, keep the reaction at the reflux temperature of 60-80°C for 6-8h; after the reaction, distill the solvent off under reduced pressure, dissolve the residue in ethanol, filter to remove triethylamine hydrochloride, pour the filtrate into a large amount of ether to precipitate The brown precipitate was filtered, washed with water several times, and vacuum-dried at 80° C. to obtain a phosphorus nitrogen oligomer flame retardant phenylphosphonamide hexamethylenediamine, with a yield of 33.0%.

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Abstract

The invention discloses a phosphorus and nitrogen oligomer flame retardant and a preparation method thereof. The preparation method of the phosphorus and nitrogen oligomer flame retardant comprises the steps: S1, respectively placing organic diamine and an acid binding agent into a solvent, and carrying out mixing to obtain a mixed solution; S2, heating the mixed solution to a reflux temperature,then, dropwise adding an activated dichlorine containing organic matter diluted by using the solvent drop by drop, and after ending the dropwise adding operation, keeping a reaction at the reflux temperature to obtain a reactant; S3, carrying out reduced pressure distillation on the reactant to remove the solvent, dissolving the solvent-removed reactant into ethanol, and carrying out filtration toremove hydrochloride to obtain filtrate; and S4, pouring the filtrate into a precipitant to separate out a brown sediment, filtering the brown sediment, washing the brown sediment with clear water, and drying the brown sediment to obtain the phosphorus and nitrogen oligomer flame retardant serving as a product. The phosphorus and nitrogen oligomer flame retardant and the preparation method thereof have the following beneficial effects that the flame retardant prepared by using the preparation method has the advantages of high thermal stability, simplicity in processing, good flame retardanceand little influences to mechanical properties of a material; and the synthesis method disclosed by the invention is simple, short in reaction time and little in reaction solvent pollution.

Description

technical field [0001] The invention relates to a phosphorus nitrogen oligomer, in particular to a phosphorus nitrogen oligomer flame retardant and a preparation method thereof. Background technique [0002] In the past 30 years, flame retardants and flame retardant polymer materials have played an important role in reducing the loss of life and property caused by fire. Although the most commonly used halogen-based flame retardants in flame retardants have incomparable high efficiency of other flame retardant series, their harm to the environment and people cannot be ignored, so halogen-free, low-smoke, low-toxic flame retardant Drugs have always been the goal pursued by people. Organophosphorus flame retardants are recognized as a variety that can replace halogenated flame retardants because of their environmental friendliness and high efficiency. [0003] At present, one of the latest research and development hotspots of halogen-free flame retardants in the world is to u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08L67/04C07F9/36C07F9/6509
CPCC07F9/36C07F9/650952C08K5/5399C08L2201/02C08L67/04
Inventor 宋平安薛逸娇俞友明
Owner ZHEJIANG FORESTRY UNIVERSITY
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