Molybdenum-containing polyoxometallate reactive flame retardant and preparation method thereof

A technology of polyoxometalate and reactive flame retardant, which is applied in the field of molybdenum-containing polyoxometalate reactive flame retardant and its preparation, can solve the problem of low flame retardant efficiency, polyoxometalate Problems such as poor compatibility of processable substrates, to improve the flame retardant effect, avoid adverse effects, and solve the effect of poor processability

Active Publication Date: 2018-12-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of molybdenum-containing polyoxometalate reactive flame retardant and its preparation method which is easy to obtain, low in price and excellent in flame retardant performance, so as to improve the low flame retardant efficiency of single element flame retardants, multi-metal Oxygen salt processability and poor compatibility with the matrix

Method used

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  • Molybdenum-containing polyoxometallate reactive flame retardant and preparation method thereof
  • Molybdenum-containing polyoxometallate reactive flame retardant and preparation method thereof
  • Molybdenum-containing polyoxometallate reactive flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {MnMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.244g p-Hydroxybenzaldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75 ℃ for 5h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 12h; concentrated under pressure, precipitated in ethyl acetate, and the product after suction filtration was dissolved in 25 mL of acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid was precipitated, filtered by suction, and dried in a vacuum to obtain the molybdenum-containing polysaccharide Oxygenate reactive flame retardant, as (C 19 h 15 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:

[0033]

[0034]Weigh 5g of epoxy resin E-51, heat up to 100°C, add 0.25g of the molybdenum-containing polyoxometalate reactive flame retardant obtained in Example 1, stir and dissolve,...

Embodiment 2

[0037] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {MnMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.176g 3-hydroxybutyraldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75°C for 10h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 12h; after the reaction, cool to room temperature, Concentrate under reduced pressure, precipitate in ethyl acetate, and the product after suction filtration is dissolved in 25mL acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid is precipitated, which is filtered by suction and dried in a vacuum to obtain the molybdenum-containing Polyoxometalate reactive flame retardant, as (C 16 h 17 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:

[0038]

Embodiment 3

[0040] Under nitrogen protection, add reactant 1.886g [(n-Bu) 4 N] 3 {FeMo 6 o 18 [(OCH 2 ) 3 CNH 2 ] 2} (1mmol), 0.176g 3-hydroxybutyraldehyde (2mmol) and 40mL acetonitrile solvent, after reflux reaction at 75°C for 5h, then add 0.54g DOPO (2.5mmol) to keep the temperature and continue the reaction for 24h; after the reaction, cool to room temperature, Concentrate under reduced pressure, precipitate in ethyl acetate, and the product after suction filtration is dissolved in 25mL acetonitrile solvent, and after slowly precipitating in ether vapor, an orange solid is precipitated, which is filtered by suction and dried in a vacuum to obtain the molybdenum-containing Polyoxometalate reactive flame retardant, as (C 16 h 17 o 3 P) 2 [(C 4 h 9 ) 4 N] 3 (MnMo 6 o 18 )[(OCH 2 ) 3 CNH] 2 , the specific structural formula is:

[0041]

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Abstract

The invention discloses a molybdenum-containing polyoxometallate reactive flame retardant and a preparation method thereof, and the molybdenum-containing polyoxometallate reactive flame retardant containing three elements of phosphorus, nitrogen and molybdenum is prepared from a molybdenum polyoxometallate having an Anderson structure, a hydroxyl aldehyde compound and DOPO as starting materials bya polyoxometallate organic modification method by organic covalent bond connection. The polyoxometallate and the DOPO are connected by means of a covalent bond, and a new function is given to the molybdenum-containing polyoxometallate reactive flame retardant while solving of the poor processability and the poor compatibility of the polyoxometallate with a matrix. The flame retardant contains a plurality of reactive groups, has good compatibility with the matrix, and can effectively avoid the adverse effects on the mechanical properties of the matrix when the polyoxometallate is added alone;by introducing of the molybdenum polyoxometallate into the flame retardant, the thermal stability of the flame retardant, the carbonization rate of the matrix resin, and the smoke suppression efficiency are remarkably improved; the preparation method is simple and easy.

Description

technical field [0001] The invention relates to the field of organic-inorganic hybrid flame retardants, in particular to a molybdenum-containing polyoxometalate reactive flame retardant and a preparation method thereof. Background technique [0002] The rapid development of transportation, electronic appliances, automobiles, engineering and other fields has made polymers such as polyurethane, polyester PET, PBT and epoxy resin widely used in the above fields. As the safety and reliability of polymers are increasingly required in these fields, the performance of polymers, especially the requirements for flame retardancy, is particularly important. Phosphorus-based flame retardants such as phosphophenanthrene derivatives have attracted widespread attention due to their environmental protection and high efficiency. Recent studies have found that adding metal elements to flame retardants can greatly improve the flame retardancy of materials. [0003] Polyoxometalates (Polyoxom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5313C08L75/04C08L67/02C08L63/00
CPCC07F9/657172C08K5/5313C08L2201/02C08L75/04
Inventor 戴李宗彭超华陈婷刘玲陈国荣曾碧榕许一婷罗伟昂袁丛辉
Owner XIAMEN UNIV
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