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A kind of flame retardant containing polyvalent phosphorus element and preparation method thereof

A phosphorus element, multivalent technology, applied in the field of phosphorus-containing flame retardants, can solve the problems to be further improved, and achieve the effect of high flame retardant efficiency

Active Publication Date: 2020-08-28
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of phosphorus-based flame retardants mainly focuses on compounds containing single-valent phosphorus elements, and there are few reports on flame retardants containing multi-valent phosphorus elements.
Hu Yuan's research group at the University of Science and Technology of China introduces phosphorus elements in different valence states into the same flame retardant structure, which can simultaneously exert the condensed phase and gas phase flame retardant mechanisms, and has a synergistic flame retardant effect (Industrial & Engineering Chemistry Research 2017, 56, 1245-1255), However, when the added amount of the flame retardant is more than 5.7%, it can pass the UL-94 vertical burning test V-0 level, and its flame retardant efficiency needs to be further improved

Method used

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  • A kind of flame retardant containing polyvalent phosphorus element and preparation method thereof
  • A kind of flame retardant containing polyvalent phosphorus element and preparation method thereof
  • A kind of flame retardant containing polyvalent phosphorus element and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] ①Trephthalaldehyde reacts with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a molar ratio of 1:2 under nitrogen protection in toluene solvent by heating to reflux temperature After 3 hours, the solvent was removed by rotary evaporation to give the phosphorus-containing diol.

[0029] 2. The above-mentioned phosphorus-containing diol, triethylamine, and diphenyl chlorophosphate were heated to 60° C. in a toluene solvent at a reaction molar ratio of 1:2:2, reacted for 24 hours, filtered, and the solvent was removed by rotary evaporation to obtain the target Product a, whose chemical structure is shown below:

[0030]

[0031] The target product a was subjected to Fourier transform infrared spectroscopy (FT-IR), hydrogen nuclear magnetic resonance spectroscopy ( 1 H-NMR) characterization, confirmed its chemical structure as follows: FT-IR (KBr, cm -1 ): 754,934(P-O-C),1226-1201(P=O),1589(P-O-Ph). 1 H-NMR (400MHz, DMSO-d 6 , ppm): 5.40–5.13 (m, 2H, (P-CH-O) ...

Embodiment 2

[0033] ①Terephthalaldehyde and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, in a molar ratio of 1:2.2, were heated to reflux temperature in toluene solvent under argon protection The reaction was carried out for 6 hours, and the solvent was removed by rotary evaporation to obtain a phosphorus-containing diol.

[0034] ②The above-mentioned phosphorus-containing diol, triethylamine, and diphenylphosphinic acid chloride were heated to 100° C. in a toluene solvent at a reaction molar ratio of 1:2.2:2.2, reacted for 6 hours, filtered, and the solvent was removed by rotary evaporation to obtain the target Product b, the chemical structure of which is shown below:

[0035]

[0036] The target product b was subjected to Fourier transform infrared spectroscopy (FT-IR), hydrogen nuclear magnetic resonance spectroscopy ( 1 H-NMR) characterization, confirm its chemical structure as follows: FT-IR (KBr, cm-1): 932 (P-O-C), 1192 (P=O), 1589 (P-Ar). 1 H-NMR (400MHz, DMSO-d 6 , p...

Embodiment 3

[0038] ①Terephthalaldehyde and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, in a molar ratio of 1:2.1, were heated to reflux temperature in toluene solvent under the protection of helium gas The reaction was carried out for 4 hours, and the solvent was removed by rotary evaporation to obtain a phosphorus-containing diol.

[0039] ②The above phosphorus-containing diol, triethylamine and chlorodiphenylphosphine were heated to 80°C in a toluene solvent at a reaction molar ratio of 1:2.1:2.1, reacted for 12 hours, filtered, and the solvent was removed by rotary evaporation to obtain the target The product c, whose chemical structure is shown below:

[0040]

[0041] The target product c was subjected to Fourier transform infrared spectroscopy (FT-IR), hydrogen nuclear magnetic resonance spectroscopy ( 1 H-NMR) characterization, confirmed its chemical structure as follows: FT-IR (KBr, cm -1 ): 932(P-O-C), 1231(P=O), 1592cm -1 (P-Ar). 1 H-NMR (400MHz, DMSO-d 6 , ppm):...

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Abstract

The invention discloses a flame retardant containing multivalent phosphorus element and a preparation method thereof. A chemical structure of the flame retardant containing multivalent phosphorus element is as shown in a formula (I), wherein R1 and R2 are respectively phosphorus-containing structures with different valence states. The chemical structure of the flame retardant containing multivalent phosphorus element simultaneously contains a plurality of phosphorus atoms with different valence states, a condensed phase flame retardant mechanism can be exerted to promote carbon formation of apolymer in a combustion process, and a gas phase flame retardant mechanism can be also exerted to captures active radicals in the combustion process. The phosphorus content and the number of aromaticrings can be adjusted, so that the flame retardant is suitable for flame retardant treatment of different polymer matrices. A limit oxygen index of epoxy resin treated with the flame retardant is obviously increased, the vertical burning grade is up to V-0 grade, and the flame retardant has the advantages of good carbon formation property, high flame retardant efficiency and the like.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame retardants, in particular to a flame retardant containing polyvalent phosphorus elements and a preparation method thereof. Background technique [0002] Phosphorus-based flame retardants, as a kind of high-efficiency, low-smoke, and low-toxicity flame retardants, have become one of the research hotspots in the field of halogen-free flame retardant technology in recent years. The flame retardant mechanisms of phosphorus-based flame retardants mainly include condensed phase and gas phase flame retardant mechanisms. In the condensed phase, the phosphorus-based flame retardant is thermally decomposed to form acidic compounds such as polymetaphosphoric acid, which catalyzes the dehydration, cyclization and carbonization of the polymer, and forms a barrier carbon layer on the surface of the polymer to prevent heat and material exchange; in the gas phase , phosphorus-based flame reta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C07F9/53C07F9/40C08L63/00C08K5/5313C08K5/5377C08K5/5397C08K5/5333C08K5/5398
CPCC07F9/4075C07F9/4084C07F9/5325C07F9/657172C08K5/5313C08K5/5333C08K5/5377C08K5/5397C08K5/5398C08L2201/02C08L63/00
Inventor 王鑫胡源宋磊郭文文邢伟义
Owner UNIV OF SCI & TECH OF CHINA
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