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Reaction type copolymerized flame-retardant furan-based polyester and preparation method thereof

A furan-based polyester, copolymerized flame-retardant technology, applied in the field of polyester and its preparation, can solve the problem of furandicarboxylic acid-based polyester being flammable

Inactive Publication Date: 2018-06-15
芜湖万隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the flammable problem of existing furandicarboxylic acid-based polyesters, and provide a reactive copolymerized flame-retardant furyl polyester and its preparation method

Method used

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  • Reaction type copolymerized flame-retardant furan-based polyester and preparation method thereof
  • Reaction type copolymerized flame-retardant furan-based polyester and preparation method thereof
  • Reaction type copolymerized flame-retardant furan-based polyester and preparation method thereof

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preparation example Construction

[0042] The present invention also provides a preparation method of reactive copolymerized flame-retardant furyl polyester, the method comprising:

[0043] Step 1: React the reactive phosphorus-containing flame retardant, diol and catalyst under nitrogen atmosphere at 150-200°C for 0.5-3 hours, preferably at 150-160°C for 1-2 hours, to obtain a prepolymerization solution;

[0044] Step 2: Under a nitrogen atmosphere, add furandicarboxylic acid or dimethyl furandicarboxylate to the prepolymerization solution obtained in step 1, react at 180-280°C for 0.5-3h, and react at 210-250°C for 2-3h to obtain a prepolymer ;

[0045] Step 3: Vacuumize the reaction system to -0.06~0.1MPa, preferably 0.09~0.1MPa, react the prepolymer obtained in step 2 at 180~280°C for 2~8h, and react at 220~250°C for 6~8h to obtain the reactive type Copolymerized flame retardant furyl polyester.

[0046] Because the phosphorus-containing dibasic acid is unstable at high temperature, the method of esterify...

Embodiment 1

[0049] (1) 20 parts of flame retardant 2-carboxyethylphenyl hypophosphorous acid, 200 parts of 1,6-hexanediol, 0.1 part of butyl titanate, under the protection of nitrogen, stirred at 150oC for 2 hours to obtain a flame retardant Prepolymer;

[0050] (2) Add 100 parts of furandicarboxylic acid into the above-mentioned flame retardant prepolymer, under nitrogen atmosphere, stir and react at 235oC for 3h to generate the prepolymer;

[0051] (3) Then evacuate to -0.090MPa, and stir the above prepolymer at 235oC for 8 hours to generate flame-retardant copolyfuryl polyester.

[0052] figure 1 It is the H NMR spectrum of the copolyfuryl polyester prepared in Example 1 of the present invention.

[0053] figure 1 It shows that the present invention has successfully prepared flame-retardant copolyfuryl polyester.

[0054] The experimental results show that: the limiting oxygen index of the flame retardant copolyester prepared in Example 1 is 28, and the vertical burning test level ...

Embodiment 2

[0056] A preparation method of flame-retardant copolymerized furyl polyester, specifically comprising the following steps:

[0057](1) 25 parts of flame retardant 2-carboxyethylphenylphosphinic acid, 150 parts of 1,3-propanediol, 0.05 part of stannous octoate, under the protection of nitrogen, stirred at 160oC for 1 hour to obtain a flame retardant prepolymer ;

[0058] (2) Add 100 parts of furandicarboxylic acid into the above-mentioned flame retardant prepolymer, under nitrogen atmosphere, stir and react at 250oC for 2h to generate the prepolymer;

[0059] (3) Then evacuate to -0.095MPa, and stir the above-mentioned prepolymer at 250°C for 6 hours to generate flame-retardant co-polyfuryl polyester.

[0060] The experimental results show that the limiting oxygen index of the flame-retardant copolyester prepared in Example 2 is 29, and the vertical burning test grade reaches UL94V-2 grade.

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Abstract

The invention provides reaction type copolymerized flame-retardant furan-based polyester and a preparation method thereof, belonging to the fields of polyester and a preparation method thereof. The polyester is prepared from the following raw materials in parts by weight: 30 to 100 parts of furandicarboxylic acid or dimethyl furandicarboxylate, 30 to 300 parts of dihydric alcohol, 0.3 to 200 partsof a reaction type phosphorus-containing flame retardant and 0.001 to 0.1 part of a catalyst. The invention also provides a preparation method for the reaction type copolymerized flame-retardant furan-based polyester. According to the invention, the reaction type phosphorus-containing flame retardant is introduced into the main chain of furan-based polyester, so obtained flame-retardant copolymerized furan-based polyester has a limit oxygen index of 30% or above, and has small addition amount, little influence on performances of substrate polyester, and long-lasting flame-retardant effect.

Description

technical field [0001] The invention belongs to the field of polyester and its preparation method, and in particular relates to a reactive copolymerized flame-retardant furyl polyester and its preparation method. Background technique [0002] Due to the shortage of petroleum resources, bio-based polyesters have attracted more and more attention. Among them, bio-polyesters synthesized from furandicarboxylic acid or dimethyl furand with various diols (2-12 carbon atoms) have been It is widely synthesized, but because of its low limiting oxygen index, it belongs to flammable polyester and has potential safety hazards. Therefore, the development of related flame-retardant biopolyesters has become a research hotspot. [0003] Patented technology, CN1267475C uses 2-carboxyethylphenylphosphinic acid (CEPPA) to react flame-retardant nylon 66, achieving permanent flame-retardant effect. CN1396206A adopts 9,10-dihydro-9-oxa-10-phosphophenanthrene-succinic acid (DDP) and 2-carboxyeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/688C08G63/78
CPCC08G63/6886C08G63/78
Inventor 周光远姜敏王国强张强王瑞
Owner 芜湖万隆新材料有限公司
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