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N-phosphorus compound-substituted phosphinimine type fire retardant and preparation method thereof

A technology of phosphinimine type and phosphorus compound is applied in the field of N-phosphorus compound substituted phosphine imine type flame retardant and its preparation. Efficient effect

Pending Publication Date: 2019-09-27
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nitrogen atoms in phosphinimines can be replaced by phosphorus compounds to form a -P=N-P- structure, but there are few reports on such compounds

Method used

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  • N-phosphorus compound-substituted phosphinimine type fire retardant and preparation method thereof
  • N-phosphorus compound-substituted phosphinimine type fire retardant and preparation method thereof
  • N-phosphorus compound-substituted phosphinimine type fire retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Diphenyl phosphite, trimethyl phosphite and sodium azide were dispersed in the solvent acetonitrile according to the molar ratio of 1:1:1.2, heated to 60°C under the protection of nitrogen, and then added dropwise tetrachloride within 2 hours. Carbonization (with a mol ratio of 1:1 to diphenyl phosphite), continued the reaction for 6 hours; the obtained reactant was washed with water, and the organic phase was dried with anhydrous magnesium sulfate to remove the organic solvent, to obtain the target product a, which The chemical structure is shown below:

[0031]

[0032] 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 ):3043(C aryl -H),2855(C alkyl -H),1592,1490(C aryl =C aryl ), 1292(P=N), 1196(P=O), 1048(=C aryl -H in-plane def.). 1 H-NMR (400MHz, CDCl 3 ,ppm):3.39-3.93(m,9H),6.7...

Embodiment 2

[0034] Diphenyl phosphite, trimethyl phosphite and sodium azide were dispersed in the solvent acetonitrile according to the molar ratio of 1:1:1.5, heated to 80°C under the protection of argon, and then added dropwise within 1 hour. Carbon chloride (1:1 molar ratio to diphenyl phosphite), and the reaction was continued for 4 hours. The obtained reactant is washed with water, the organic phase is dried with anhydrous magnesium sulfate, and the organic solvent is removed to obtain the target product a.

Embodiment 3

[0036] Diphenyl phosphite, trimethyl phosphite and sodium azide were dispersed in the solvent acetonitrile according to the molar ratio of 1:1:2, heated to 82°C under the protection of helium gas, and then added dropwise within 0.5 hours. Carbon chloride (1:1 molar ratio to diphenyl phosphite), and the reaction was continued for 2 hours. The obtained reactant is washed with water, the organic phase is dried with anhydrous magnesium sulfate, and the organic solvent is removed to obtain the target product a.

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Abstract

The invention discloses an N-phosphorus compound-substituted phosphinimine type fire retardant and a preparation method thereof; the chemical structure of the N-phosphorus compound-substituted phosphinimine type fire retardant is shown as a formula (I); the formula (I) is shown in the description, wherein R1 and R2 are respectively any one of methoxy group, oxyethyl group, phenoxy group and phenyl group. Phosphorus atoms and nitrogen atoms are simultaneously included in the chemical structure of the the N-phosphorus compound-substituted phosphinimine type fire retardant, a phosphorus-nitrogen synergistic fire retardant effect can be exerted, and the fire retardant efficiency is high; phosphorus content and aromatic ring amount can be adjusted, and the fire retardant is suitable for fire retardant treatment of different polymer matrices. The limit oxygen index of epoxy resin treated by the fire retardant disclosed by the invention reaches 30%, and the vertical burning grade reaches V-0 grade; the fire retardant has the advantages of good char-forming property, high fire retardant efficiency, good compatibility with the matrices and the like.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame retardants, in particular to an N-phosphorus compound substituted phosphinimine type flame retardant 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 mechanism of phosphorus-based flame retardants mainly includes thermal decomposition to form acidic compounds such as polymetaphosphoric acid, catalyzing polymer dehydration, cyclization, and carbonization, forming a barrier carbon layer on the surface of the polymer, preventing heat and material exchange, so as to achieve The purpose of preventing burning. At present, the commercial halogen-free phosphorus flame retardants mainly include ammonium polyphosphate, hypophosphit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C07F9/24C07F9/535C08L63/00
CPCC07F9/2454C07F9/5355C08K5/5399C08L2201/02C08L63/00
Inventor 王鑫胡源宋磊郭文文
Owner UNIV OF SCI & TECH OF CHINA