Flame retardant containing multivalent phosphorus element and preparation method thereof

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

Active Publication Date: 2019-09-13
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Flame retardant containing multivalent phosphorus element and preparation method thereof
  • Flame retardant containing multivalent phosphorus element and preparation method thereof
  • Flame retardant containing multivalent phosphorus element and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0029] ②Heat the above phosphorus-containing dihydric alcohol, triethylamine, and diphenyl chlorophosphate to 60°C in toluene solvent according to the reaction molar ratio of 1:2:2, react for 24 hours, filter, and remove the solvent by rotary evaporation to obtain the target Product a, its chemical structure is as follows:

[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 that its chemical structure is 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) 2 ),8.27-8.13...

Embodiment 2

[0033] ① Heat terephthalaldehyde and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a molar ratio of 1:2.2 in toluene solvent to reflux temperature under the protection of argon After reacting for 6 hours, the solvent was removed by rotary evaporation to obtain phosphorus-containing dihydric alcohol.

[0034] ②Heat the above phosphorus-containing dihydric alcohol, triethylamine, and diphenylphosphinoyl chloride in toluene solvent to 100°C according to the reaction molar ratio of 1:2.2:2.2, react for 6 hours, filter, and remove the solvent by rotary evaporation to obtain the target Product b, its chemical structure 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, confirmed that its chemical structure is as follows: FT-IR (KBr, cm-1): 932 (P-O-C), 1192 (P=O), 1589 (P-Ar). 1 H-NMR (400MHz, DMSO-d 6 ,ppm):5.41–5.16(m,2H,...

Embodiment 3

[0038] ① Heat terephthalaldehyde and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a molar ratio of 1:2.1 in toluene solvent to reflux temperature under the protection of helium After reacting for 4 hours, the solvent was removed by rotary evaporation to obtain phosphorus-containing dihydric alcohol.

[0039] ②Heat the above-mentioned phosphorus-containing dihydric alcohol, triethylamine, and chlorinated diphenylphosphine to 80°C in toluene solvent according to the reaction molar ratio of 1:2.1:2.1, react for 12 hours, filter, and remove the solvent by rotary evaporation to obtain the target Product c, its 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 that its chemical structure is 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, and in particular relates to a flame retardant containing polyvalent phosphorus elements and a preparation method thereof. Background technique [0002] As a high-efficiency, low-smoke, and low-toxicity flame retardant, phosphorus-based flame retardants have become one of the research hotspots in the field of halogen-free flame retardant technology in recent years. The flame retardant mechanism of phosphorus-based flame retardants mainly includes condensed phase and gas phase flame retardant mechanisms. In the condensed phase, the phosphorus-based flame retardant is decomposed by heat 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 ret...

Claims

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Application Information

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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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