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Phosphorus-containing Schiff base structured flame retardant and preparation method thereof

A structural flame retardant, Schiff base technology, applied in the field of polymer science, can solve the problems of easy aging, decomposition and migration, reducing the effect of flame retardants, poor thermal stability, etc., and achieves good application prospects, good flame retardant effect, phase Good capacitive effect

Active Publication Date: 2016-10-12
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent CN103073727A discloses a preparation method of a linear flame retardant containing a Schiff base structure, which has a relatively low molecular weight, poor thermal stability, and is easy to age and decompose and migrate out of the matrix, which not only reduces the effect of the flame retardant , and its decomposition products may pollute the environment

Method used

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  • Phosphorus-containing Schiff base structured flame retardant and preparation method thereof
  • Phosphorus-containing Schiff base structured flame retardant and preparation method thereof
  • Phosphorus-containing Schiff base structured flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] 1. Add 0.5mol ethylenediamine to a flask equipped with a hydrogen chloride absorption device, and 0.1mol phenylphosphoryl chloride (R 4 H) Slowly add it dropwise to ethylenediamine, heat to 40°C for 1 hour under stirring and react for 1 hour, a light yellow precipitate is formed, distill under reduced pressure, recover excess ethylenediamine, wash with alcohol, and dry under vacuum at 60°C to obtain a viscous product containing Phosphorus diamine, its structural formula is as follows:

[0042]

[0043] 2. Take 0.05mol phosphorus-containing diamine and ultrasonically disperse it in ethanol, add 0.1mol p-hydroxybenzaldehyde dissolved in ethanol drop by drop, and react at 60°C for 3 hours after dropping, a light yellow precipitate is formed, suction filter, vacuum at 60°C Dried to obtain phosphorus-containing dihydric phenol containing Schiff base structure, its structural formula is as follows:

[0044]

[0045] 3. Disperse 0.03 mol of dihydric phenol containing ph...

Embodiment 2

[0052] 1. Add 0.5mol ethylenediamine to a flask equipped with a hydrogen chloride absorption device, and 0.1mol phenylphosphoryl chloride (R 4 H) Slowly add it dropwise to ethylenediamine, heat it to 40°C for 2 hours under stirring, and react for 2 hours, a light yellow precipitate is formed, distill under reduced pressure, recover excess ethylenediamine, wash with alcohol, and dry under vacuum at 60°C to obtain a viscous product containing Phosphorus diamine, its structural formula is as follows:

[0053]

[0054] 2. Take 0.05mol phosphorus-containing diamine and ultrasonically disperse it in ethanol, add 0.1mol p-hydroxybenzaldehyde dissolved in ethanol drop by drop, and react at 60°C for 3 hours after dropping, a light yellow precipitate is formed, suction filter, vacuum at 60°C Dried to obtain phosphorus-containing dihydric phenol containing Schiff base structure, its structural formula is as follows:

[0055]

[0056] 3. Disperse 0.03mol of dihydric phenol containi...

Embodiment 3

[0063] 1. Add 0.25mol of p-nitrophenol to dissolve in tetrahydrofuran in a flask equipped with a hydrogen chloride absorption device, add 0.22mol of triethylamine as an acid agent, 0.002mol of copper chloride as a catalyst, and dissolve 0.1mol of phenylphosphoryl chloride (R 4 H) very slowly drop into the mixture, react at 40°C for 24 hours, disperse the product in water, use 0.005mol tin protochloride as a catalyst, adjust the pH value to 5 with hydrochloric acid, react at 80°C for 24 hours, after suction filtration Phosphorus-containing diamine can be prepared by drying, and its structural formula is as follows:

[0064]

[0065] 2. Ultrasonic disperse 0.05 mol of the prepared phosphorus-containing diamine in ethanol, add 0.1 mol of p-hydroxybenzaldehyde dissolved in ethanol drop by drop, reflux at 70°C for 4 hours, obtain precipitate, suction filter, and vacuum dry at 60°C. Promptly obtain the dihydric phenol containing phosphorus containing Schiff base structure, its s...

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Abstract

The invention discloses a phosphorus-containing Schiff base structured flame retardant and a preparation method thereof. The phosphorus-containing Schiff base structured flame retardant consists of hyperbranched macromolecules; a hyperbranched repeat unit is shown in the formula (I) as shown in the specification; in the formula, R1 is a phosphorus-containing structure, and R2 is a trifunctional structure; the molecular weight of the flame retardant is 500-100000. The flame retardant disclosed by the invention consists of hyperbranched macromolecules and is relatively large in molecular weight; when the flame retardant is used in polyurethane foams, the carbon residue amount of polyurethane can be greatly increased; the flame retardant disclosed by the invention is free of halogen and is a green and environment-friendly flame retardant; the flame retardant contains substances of a Schiff base structure, and due to existence of a C=N structure, very important chemical and biological significances can be achieved due to lone pair electrons on N atoms.

Description

1. Technical field [0001] The invention relates to a hyperbranched green flame retardant and a preparation method thereof, in particular to a phosphorus-containing Schiff base structure flame retardant and a preparation method thereof, belonging to the field of polymer science and technology. 2. Background technology [0002] Halogen-free organic flame retardants are mainly flame retardants containing phosphorus and nitrogen. It also overcomes the disadvantage of causing suffocation of personnel, and also overcomes the adverse effects of inorganic flame retardants on material mechanics and processing properties due to large additions. Schiff base structure Due to the existence of the C=N structure, the lone pair of electrons on the N atom endows it with very important chemical applications. During the pyrolysis process, it can neutralize active free radicals in the gas phase; during the pyrolysis process, phosphorus-containing compounds not only It will decompose PO free ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08L75/08C08L87/00
CPCC08G83/005C08L75/08C08L2201/02C08L2201/08C08L2203/14C08L87/00
Inventor 胡伟兆侯雁北宋磊胡源阚永春
Owner UNIV OF SCI & TECH OF CHINA
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