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A kind of long-chain metal coordination expansion flame retardant and preparation method thereof

An intumescent flame retardant and metal coordination technology, which is applied in the field of long-chain metal coordination intumescent flame retardant and its preparation, can solve the damage of material mechanical properties and processing properties, and the processing and recycling of flame retardant polymers difficult, low flame retardant efficiency and other problems, to achieve the effect of high yield, simple product post-processing, and easy operation

Inactive Publication Date: 2016-04-27
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with halogen-based flame retardants, inorganic flame retardants based on endothermic flame retardants and intumescent flame retardants (IFR) based on condensed phase flame retardants are currently recognized as environmentally friendly "green flame retardants" by the scientific and industrial circles. "Flame retardants, but this kind of flame retardants often need a higher amount of addition to make the material achieve the expected flame retardant effect, the flame retardant efficiency is low, and the mechanical properties and processing properties of the material are greatly damaged. At the same time, Poor thermal stability and low decomposition temperature cause difficulties in the processing and recycling of flame-retardant polymers

Method used

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  • A kind of long-chain metal coordination expansion flame retardant and preparation method thereof
  • A kind of long-chain metal coordination expansion flame retardant and preparation method thereof
  • A kind of long-chain metal coordination expansion flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 250ml four-necked flask equipped with a magnetic stirrer, a thermometer, and a spherical condenser, add 0.2mol of phosphorous acid, 100ml of concentrated hydrochloric acid, and polyethyleneimine (1mmol) with a degree of polymerization of 100, heat to reflux under stirring, and take 37% of Add 32ml of formaldehyde solution to the flask dropwise within 1 hour. The reaction was then continued for 2 h at reflux temperature. After the reaction, cool to room temperature and neutralize to neutral with ethylene glycol amine, wash with absolute ethanol three times, and filter to obtain the product with structural formula (II), with a yield of 95%). The compound with structural formula (II), namely PEIP (0.53mmol), zinc acetate (0.1mol), sodium hydroxide 0.05mol, and absolute ethanol 500ml, was stirred and heated to reflux for 7 hours, filtered and washed three times with absolute ethanol, filtered Obtaining structural formula is the product (the infrared spectrum of struct...

Embodiment 2

[0028] In a 250ml four-neck flask equipped with a magnetic stirrer, a thermometer and a spherical condenser, add 0.2mol of phosphorous acid, 100ml of concentrated hydrochloric acid, and a degree of polymerization of 100 polyethyleneimine (1mmol), heat and reflux under stirring, and take 37% formaldehyde aqueous solution 32ml, dropwise into the flask within 1h. The reaction was then continued for 2 h at reflux temperature. After the reaction, cool to room temperature, neutralize to neutral with ethylene glycol amine, wash with absolute ethanol three times, and filter to obtain the product with structural formula (II), with a yield of 95%. The compound with structural formula (II), namely PEIP (0.53mmol), manganese acetate (0.1mol), sodium hydroxide 0.05mol, and absolute ethanol 500ml, was stirred and heated to reflux for 7 hours, filtered and washed three times with absolute ethanol, filtered Obtaining structural formula is the product of (I) (the infrared spectrogram of struc...

Embodiment 3

[0031] In a 250ml four-neck flask equipped with a magnetic stirrer, a thermometer and a spherical condenser, add 0.2mol of phosphorous acid, 100ml of concentrated hydrochloric acid, and a degree of polymerization of 100 polyethyleneimine (1mmol), heat and reflux under stirring, and take 37% formaldehyde aqueous solution 32ml, dropwise into the flask within 1h. The reaction was then continued for 2 h at reflux temperature. After the reaction, cool to room temperature, neutralize to neutral with ethylene glycol amine, wash with absolute ethanol three times, and filter to obtain the product with structural formula (II), with a yield of 95%. The compound with structural formula (II), namely PEIP (0.53mmol), cobalt acetate (0.1mol), sodium hydroxide 0.05mol, and absolute ethanol 500ml, was stirred and heated to reflux for 7 hours, filtered and washed three times with absolute ethanol, filtered Obtaining structural formula is the product of (I) (the infrared spectrogram of structur...

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Abstract

The invention discloses a long-chain type metal coordination intumescent flame retardant and a preparation method thereof. The preparation method comprises the following steps of: synthesizing a long-chain type intermediate product simultaneously containing phosphorus and nitrogen elements by using polyethyleneimine, formaldehyde and phosphorous acid as raw materials; performing coordination reaction on the long-chain type intermediate product and metal acetate to obtain the long-chain type metal coordination intumescent flame retardant. The synthesis method is simple in process, easy for reaction operation and suitable for industrial production, and has low-cost and easily-available raw materials; the flame retardant does not contain halogen and belongs to the green environment-friendly flame retardant; the structural formula is shown as the formula (I) in the specification.

Description

technical field [0001] The invention relates to a long-chain metal coordination expansion flame retardant and a preparation method thereof. It specifically relates to a halogen-free, environmentally friendly intumescent flame retardant used in the field of flame retardants and a preparation method thereof. Background technique [0002] In recent years, the research and development of flame-retardant materials has become increasingly active all over the world, and various flame-retardant products have come out continuously. Halogenated flame retardants, mainly gas-phase flame retardants, have good flame retardant effects, but they release toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment. For this reason, in the two directives of the "Waste Electrical and Electronic Equipment Directive" (WEEE) and the "Directive on the Prohibition of Hazardous Substances in Electrical and Electronic Equipment" (RoHS) promulgated by th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/04
Inventor 张艳方征平李晓楠曹贞虎
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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