Phosphorus-containing Schiff base derivative intumescent fire retardant and preparation method thereof

A technology of intumescent flame retardant and Schiff base, which is applied in the field of phosphorus-containing Schiff base derivative intumescent flame retardant and its preparation, can solve the problem of material mechanical properties and processing performance damage, thermal decomposition temperature limit application, resistance problems such as the decline in fuel efficiency, and achieve the effects of good application prospects, easy control, and high carbon formation.

Inactive Publication Date: 2012-10-17
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the addition of inorganic flame retardants such as aluminum hydroxide or magnesium hydroxide is high, and the flame retardant efficiency is low, which greatly damages the mechanical properties and processing properties of the material; although the flame retardant of the intumescent flame retardant Good performance, low addition amount, but low thermal decomposition temperature limits its application in engineering plastics, and its small molecular weight can easily cause matrix migration during use, which can easily lead to a decrease in flame retardant efficiency

Method used

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  • Phosphorus-containing Schiff base derivative intumescent fire retardant and preparation method thereof
  • Phosphorus-containing Schiff base derivative intumescent fire retardant and preparation method thereof
  • Phosphorus-containing Schiff base derivative intumescent fire retardant and preparation method thereof

Examples

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Effect test

Embodiment 1

[0045] Add 20mmol of p-hydroxybenzaldehyde and 100ml of absolute ethanol in a 250ml flask, heat to 50°C under stirring, then dissolve 10mmol of diethylenetriamine in 100ml of absolute ethanol, slowly drop into the flask, and continue the reaction for 2h. After cooling to room temperature, a large amount of yellow solids precipitated, filtered with suction, washed three times with absolute ethanol and deionized water, precipitated with deionized water, and dried in a vacuum oven to obtain the product DDBHA with general structural formula (II) (infrared spectrum See figure 1 ). Add 5mmol DDBHA, 10mmol NaOH, 0.05mmol of phase transfer catalyst tetrabutylammonium bromide and 25ml of deionized water into the three-necked flask, mechanically stir at 25°C to completely dissolve DDBHA, then quickly add benzene dichlorinated phosphate 25ml of the dichloromethane solution of the ester was stirred quickly, and after 1 hour of reaction, the product was suction filtered, rinsed with a lar...

Embodiment 2

[0051] Add 20mmol of p-hydroxybenzaldehyde and 100ml of absolute ethanol in a 250ml flask, heat it to 50°C under stirring, then slowly add 10mmol of ethylenediamine and 100ml of absolute ethanol dropwise into the flask, continue the reaction for 1h, and cool to room temperature A large amount of yellow solids were precipitated, filtered by suction, washed three times with absolute ethanol and deionized water respectively, precipitated with deionized water, and dried in a vacuum oven to obtain the product EDBHA with the general structure formula (II) (infrared spectrum see image 3 ). Add 5mmol EDBHA, 10mmol NaOH, 0.05mmol of phase transfer catalyst tetrabutylammonium chloride and 25ml of deionized water into the three-necked flask, mechanically stir at 25°C to completely dissolve the EDBHA, then quickly add benzene dichlorinated phosphate 25ml of the dichloromethane solution of the ester was stirred quickly, and after 1 hour of reaction, the product was suction-filtered, rinse...

Embodiment 3

[0057] Add 20mmol of p-hydroxybenzaldehyde and 100ml of absolute ethanol in a 250ml flask, heat to 50°C under stirring, then slowly add 10mmol of p-phenylenediamine and 100ml of absolute ethanol dropwise into the flask, continue the reaction for 3h, and cool to A large number of yellow solids precipitated at room temperature, filtered by suction, washed three times with absolute ethanol and deionized water, precipitated with deionized water, and dried in a vacuum oven to obtain the product PDBHA with the general structural formula (II) (infrared spectrum see Figure 5 ). Add 5mmol PDBHA, 10mmol NaOH, 0.05mmol of phase transfer catalyst tetrabutylammonium chloride and 25ml of deionized water into the three-necked flask, mechanically stir at 25°C to dissolve all the PDBHA, then quickly add benzene dichlorinated phosphate 25ml of the dichloromethane solution of the ester, stirred rapidly, after reacting for 1h, the product was suction filtered, rinsed with a large amount of deion...

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Abstract

The invention discloses a phosphorus-containing Schiff base derivative intumescent fire retardant and a preparation method thereof. The method comprises the following steps: reacting hydroxy-aldehyde compounds with diamine compounds or reacting diamine compounds with hydroxy-amine compounds to obtain imine-diphenol, wherein two terminals of the molecule of imine-diphenol have phenolic hydroxyl groups and the skeleton of the imine-diphenol molecule contains a Schiff base structure; and allowing obtained diphenol Schiff base and phenyl dichlorophosphate to undergo interfacial polymerization under the action of a catalyst so as to obtain intumescent fire retardants with different phosphorus and nitrogen content. The synthetic method provided in the invention has the advantages of a simple process, easy reaction operation and suitability for industrial production; and the prepared fire retardant does not contain halogen, belonging to green environment-friendly fire retardants, and has a general structural formula as represented by formula (I).

Description

technical field [0001] The invention relates to a phosphorus-containing Schiff base derivative expansion type flame retardant and a preparation method thereof. This type of polymer can be used in the field of flame retardants, and this type of polymer does not contain halogen, and belongs to the environment-friendly flame retardant. Background technique [0002] In today's society, the voice of green environmental protection is getting higher and higher, and so is the field of flame retardancy. Inorganic flame retardants and intumescent flame retardants are environmentally friendly flame retardants recognized by the scientific and industrial circles, and have been applied in many fields. However, the addition of inorganic flame retardants such as aluminum hydroxide or magnesium hydroxide is high, and the flame retardant efficiency is low, which greatly damages the mechanical properties and processing properties of the material; although the flame retardant of the intumescen...

Claims

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Application Information

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IPC IPC(8): C08L85/02C08G79/04
Inventor 方征平刘妍张艳曹贞虎
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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