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Phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer and preparation method thereof

A flame retardant polymer, nitrogen expansion technology, applied in nitrogen expansion flame retardant polymer and its preparation, phosphorus-containing field, can solve the problem of reducing the flame retardant performance and service life of materials, not meeting the requirements of plastic processing, low decomposition temperature, etc. problems, to achieve broad industrial application prospects, good fire protection, and good compatibility

Active Publication Date: 2012-07-25
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most intumescent flame retardants have the following disadvantages: first, their decomposition temperature is low, which cannot meet the processing requirements of some plastics; Permeation and precipitation reduce the flame retardancy and service life of the material

Method used

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  • Phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer and preparation method thereof
  • Phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer and preparation method thereof
  • Phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 0.1mol diaminodiphenylmethane and 90ml anhydrous acetonitrile into a 250ml three-necked flask equipped with a stirrer, heat up to 80°C while stirring, add 0.2mol triethylamine after the solid dissolves, and then add 10ml dropwise within 1h 0.1mol phenyl phosphate dichloride dissolved in acetonitrile; after reacting for 9 hours, remove triethylamine hydrochloride by filtration while hot, remove the acetonitrile solvent by rotary evaporation, dissolve the crude product with 50ml dimethyl sulfoxide (DMSO), and wait until the product is completely After dissolving, the solution was added dropwise to 800 ml of deionized water, then suction filtered, washed and vacuum dried to obtain an off-white solid with a yield of 85%.

[0020] The obtained product was analyzed by proton nuclear magnetic resonance spectrum. The peak position of the chemical shift at 8.22-8.26ppm is the hydrogen vibration signal on the -P-NH-bond, and the peak at the chemical shift of 6.49-7.54ppm is th...

Embodiment 2

[0023] Add 0.15mol (37.2g) diaminodiphenyl sulfone and 270ml anhydrous acetonitrile into a 500ml three-neck flask equipped with a stirrer, heat up to 82°C while stirring, and add 0.30mol (30.6g) triethylamine after the solid is dissolved , then drop 0.15mol (31.65g) phenyl phosphate dichloride dissolved in 30ml of acetonitrile within 1h; Sulfoxide (DMSO) was used to dissolve the crude product. After the product was completely dissolved, the solution was added dropwise to 1500 ml of deionized water, followed by suction filtration, washing and vacuum drying to obtain an off-white solid with a yield of 80%.

[0024] The obtained product is analyzed by proton nuclear magnetic resonance spectrum. The peak position at the chemical shift of 9.0-9.5ppm is the hydrogen vibration signal on the -P-NH-bond, and the peak at the chemical shift of 6.49-8.0ppm is the hydrogen on the benzene ring. Vibration signal; nuclear magnetic resonance phosphorus spectrum shows that the chemical shift of...

Embodiment 3

[0027] Add 0.025mol (5.0g) diaminodiphenyl ether and 60ml anhydrous acetonitrile into a 50ml three-necked flask equipped with a stirrer, heat up to 82°C while stirring, and add 0.05mol (5.1g) triethylamine after the solid is dissolved , then dropwise added 0.025mol (5.28g) phenyl phosphate dichloride within 1.5h; after reacting for 7h, remove the acetonitrile solvent by rotary evaporation, dissolve the crude product with 30ml dimethyl sulfoxide (DMSO), and filter to remove undissolved Triethylamine hydrochloride, the solution was added dropwise to 600ml deionized water, then suction filtered, washed and vacuum dried to obtain a white solid.

[0028] The obtained product is analyzed by proton nuclear magnetic resonance spectrum. The peak position of the chemical shift at 8.20-8.50ppm is the hydrogen vibration signal on the -P-NH-bond, and the peak at the chemical shift of 6.50-7.60ppm is the hydrogen on the benzene ring. Vibration signal; nuclear magnetic resonance phosphorus s...

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Abstract

The invention discloses a phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer and a preparation method thereof. The preparation method is characterized in that: the phosphorus-containing and nitrogen-containing expansion type flame-retardant polymer is prepared by solution polycondensation reaction or melt polycondensation reaction of diphosphorus acylchloride or diphosphorus acylbromide and a diamine functional group-containing compound. The expansion type flame-retardant polymer comprises phosphorus-containing and nitrogen-containing phosphamide with a structure unit formula shown in the specifications, wherein n is an integer of from 1 to 200; R1 is oxygen or sulphur; and R is alkoxy, alkylthio, aryloxy or arylthio. The product of the invention has highcompatibility with a high molecular material matrix, difficult transfer and excellent durability. The preparation method has the advantages of simpleness, easy control, high yield, wide sources of the required raw materials and easy industrialized production. A high polymer with a flame-retardant function can be directly prepared, or the high polymer serving as a flame-retardant additive can be added into various polyesters, polyamide, polyolefin, epoxy resin, polystyrene, high impact polystyrene or acrylonitrile butadiene styrene (ABS) polymer.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame-retardant polymers, and in particular relates to phosphorus- and nitrogen-containing intumescent flame-retardant polymers and a preparation method thereof. Background technique [0002] Polymer materials have many advantages such as light weight, chemical corrosion resistance, easy processing and molding, wide operating temperature range, and high cost performance. They have been widely used in electronics, electrical appliances, construction and other fields and in daily life. However, because most polymer materials are composed of C, H, O and other elements, they are easy to burn and cause fires, which bring huge threats and losses to people's lives and property. [0003] At present, the industry mainly adopts the addition of halogen-containing flame retardants in the matrix of polymer materials to solve the problem of flammability of polymer materials. For example, some bromine-cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/02
Inventor 胡源台启龙宋磊
Owner UNIV OF SCI & TECH OF CHINA