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Ferrocene-dopo double base polyester flame retardant and smoke suppressant and its preparation method and application in flame retardant polymer

A ferrocene-based polyester technology is applied in the field of polymer compound flame retardants, which can solve the problems of poor compatibility of matrix materials, low carbon formation rate, and large addition amount.

Active Publication Date: 2020-07-07
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the phosphorus-based flame retardants in the prior art are small molecules, which have poor compatibility with the matrix material, large addition amount, and low char formation rate

Method used

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  • Ferrocene-dopo double base polyester flame retardant and smoke suppressant and its preparation method and application in flame retardant polymer
  • Ferrocene-dopo double base polyester flame retardant and smoke suppressant and its preparation method and application in flame retardant polymer
  • Ferrocene-dopo double base polyester flame retardant and smoke suppressant and its preparation method and application in flame retardant polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A preparation method of a ferrocene-DOPO double-base polyester type flame retardant and smoke suppressant, the steps are:

[0044] Weigh 1.6g DOPO-HQ (5mmol) into a 250ml three-neck flask with magnetic stirring, place the flask in an oil bath, measure 30ml of dichloromethane into the flask, stir for a while; add 1.4ml of triethylamine (10mmol) and continue to stir; after 10min, slowly add 20ml 1,1'-ferrocenedicarboxylic acid chloride (1.55g, 5mmol) / dichloromethane solution dropwise through the constant pressure dropping funnel; Stir the reaction for 10 hours, filter after the reaction is complete, pour the filtrate into 400ml of methanol, and immediately precipitate a large amount of yellow solid, filter it with suction, wash it with methanol for 3 times, and dry it in vacuum at 50°C for 5 hours to obtain 2.68g of yellow solid, which is the prepared Ferrocene-DOPO double base polyester flame retardant and smoke suppressant—chemical name is poly 10-(2,5-dihydroxyphenyl)-...

Embodiment 2

[0048] A preparation method of a ferrocene-DOPO double-base polyester type flame retardant and smoke suppressant, the steps are:

[0049] Weigh 1.6g DOPO-HQ (5mmol) into a 250ml three-neck flask with magnetic stirring, place the flask in an oil bath, measure 30ml N,N-dimethylformamide (DMF) into the flask, Stir for a while; add 0.4ml (5mmol) of pyridine and continue stirring; after 10min, slowly add 20ml of 1,1'-ferrocenedicarboxylic acid chloride (1.4g, 4.5mmol) / DMF solution dropwise through a constant pressure dropping funnel; , heated up to 50°C under nitrogen protection and stirred for 1 hour, filtered after the reaction was complete, poured the filtrate into 500ml of deionized water, and immediately precipitated a large amount of yellow solid, filtered it with suction, washed 3 times with deionized water, and dried it in vacuum at 80°C for 5 hours. 2.6 g of a yellow solid was obtained, which was the ferrocene-DOPO double base polyester type flame retardant and smoke suppr...

Embodiment 3

[0051]A kind of preparation method of ferrocene-DOPO double base polyester type flame retardant and smoke suppressant, the steps are: take by weighing 1.6g DOPO-HQ (5mmol) and place in a 250ml three-necked flask with magnetic stirring, place the flask in In the oil bath, measure 30ml of dichloromethane into the flask and stir for a while; add 1.73ml (12.5mmol) of triethylamine and continue stirring; after 10min, slowly add 20ml of 1,1'-di Ferrocene diacetyl chloride (2.33g, 7.5mmol) / dichloromethane solution; after dropping, reflux and stir the reaction for 5h under the protection of nitrogen at 10°C, filter after the reaction, pour the filtrate into 250ml methanol, and immediately precipitate a large amount of yellow solid, Suction filtration, washing with methanol for 3 times, vacuum drying at 40°C for 12 hours to obtain 2.7 g of a yellow solid, which is the ferrocene-DOPO double-based polyester flame retardant and smoke suppressant, with a yield of 85.7%.

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Abstract

The invention discloses a ferrocene-DOPO biradical polyester type flame retarding and smoke suppressing agent and a preparation method of the ferrocene-DOPO biradical polyester type flame retarding and smoke suppressing agent. The preparation method of the polymer is as follows: putting 10-(2,5-dyhydroxyl phenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into a reactor, adding a solvent,stirring for 5-10 minutes, adding an acid-binding agent; taking R1,R2'-ferrocene oxalyl chloride, adding the solvent, mixing, adding into the reactor dropwise, thermally insulating, stirring and reacting for 1-15 hours at the temperature of 0-50 DEG C under the protection of nitrogen after finishing adding dropwise; pouring a liquid obtained after the reaction into a precipitator while stirring, wherein the volume of the precipitator is 5-10 times that of the liquid, precipitating a yellow solid, carrying out suction filtration, washing a filter cake by using the precipitator, and drying to obtain the ferrocene-DOPO biradical polyester type flame retarding and smoke suppressing agent. The ferrocene-DOPO biradical polyester type flame retarding and smoke suppressing agent can be used to retard flame and suppress smoke of high polymer materials like polyolefins and epoxy resins.

Description

technical field [0001] The invention belongs to a high molecular compound flame retardant and its preparation and use, and relates to a ferrocene-DOPO double base polyester type flame retardant and smoke suppressant, a preparation method thereof and an application in a flame retardant polymer. The polyester flame retardant and smoke suppressant containing ferrocene and DOPO structure of the invention is suitable for flame retardant and smoke suppression in polymer materials such as epoxy resin and polypropylene. Background technique [0002] Since the 1950s, with the development of polymer materials, polymer materials have been widely used in many fields due to their unique advantages, such as the three major synthetic polymer materials: plastics, synthetic rubber, and synthetic fibers. However, most of the polymer materials are easy to burn or can burn, and during the combustion process, the calorific value of combustion is large and difficult to extinguish, and releases to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/692C08G63/68C08L63/00C08L67/02C08L23/12
CPCC08G63/681C08G63/6926C08L23/12C08L63/00C08L2201/02C08L67/02
Inventor 胡小平文溢
Owner SOUTHWEAT UNIV OF SCI & TECH
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