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Composite expandable flame retardant modified thermosetting resin and preparation method thereof

An intumescent flame retardant and composite technology, which is applied in the field of composite intumescent flame retardant modified thermosetting resin and its preparation, can solve the problem of difficult dispersibility, interfacial force, reduction of material heat resistance, influence on flame retardant performance, etc. problems, to achieve excellent thermal oxygen shielding effect, good bonding force, outstanding heat resistance and flame retardant properties.

Inactive Publication Date: 2014-02-26
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many problems with mixing the two intumescent flame retardants
First of all, physical mixing makes it difficult for physical flame retardants to obtain good dispersion and interfacial force in the organic matrix, which affects the performance of flame retardant performance
Secondly, in order to obtain a good flame retardant effect, usually chemical expansion flame retardants need to be added in a higher amount, which reduces the heat resistance of the material

Method used

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  • Composite expandable flame retardant modified thermosetting resin and preparation method thereof
  • Composite expandable flame retardant modified thermosetting resin and preparation method thereof
  • Composite expandable flame retardant modified thermosetting resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Preparation of composite intumescent flame retardant

[0027] Add 5g of 80 mesh expandable graphite and 50g of dioxane into a three-necked flask, stir and mix evenly to obtain a suspension A of expandable graphite;

[0028] Add 2.58g of phosphorus oxychloride to 25.8g of dioxane to prepare solution B. Add solution B to suspension A to obtain mixed solution C; heat mixed solution C to 40°C, and react under nitrogen protection for 2 hours to obtain reaction solution D in which phosphorus oxychloride expandable graphite is formed;

[0029] According to the molar ratio of phosphorus oxychloride and pentaerythritol as 1:1, 2.29g of pentaerythritol was added to the above reaction solution D, and 0.0046g of anhydrous stannous chloride was added; the temperature was raised to 60°C for 4 hours to obtain reaction solution E. According to the pentaerythritol and 1,3,5-triglycidyl-S-triazinetrione molar ratio of 1:1, 5.63g of 1,3,5-triglycidyl-S-triazinetrione was added to the ...

Embodiment 2

[0038] 1. Preparation of composite intumescent flame retardant

[0039] Add 5g of 100 mesh expandable graphite and 50g of dioxane into a three-necked flask, stir and mix evenly to obtain a suspension A of expandable graphite;

[0040] Add 2 g of phosphorus oxychloride to 20 g of dioxane to prepare solution B. Add solution B to suspension A to obtain mixed solution C; heat mixed solution C to 50° C., and react under nitrogen protection for 1 hour to obtain reaction solution D in which phosphorus oxychloride expandable graphite is formed;

[0041] According to the molar ratio of phosphorus oxychloride and pentaerythritol as 1:1, 1.03g of pentaerythritol was added to the above reaction solution D, and 0.0021g of anhydrous stannous chloride was added; the temperature was raised to 70°C for 3 hours to obtain reaction solution E. According to the pentaerythritol and 1,3,5-triglycidyl-S-triazinetrione molar ratio of 1:1.5, 5.82g of 1,3,5-triglycidyl-S-triazinetrione was added to the...

Embodiment 3

[0047] 1. Preparation of composite intumescent flame retardant

[0048] Composite intumescent flame retardant was prepared according to Example 2.

[0049] 2. Preparation of composite intumescent flame retardant modified cyanate resin and its cured product

[0050] Weigh 10g of composite intumescent flame retardant and 90g of bisphenol A cyanate, stir and mix them at 80°C to obtain a composite intumescent flame retardant-modified cyanate resin.

[0051] Pour the obtained composite intumescent flame retardant modified cyanate ester resin into a preheated mold, and vacuum defoam at 150°C for 1 hour. o C / 2h+200 o C / 2h+220 o The process of C / 2h is solidified, and after natural cooling, the mold is demoulded, and the solidified composite intumescent flame retardant modified cyanate ester resin is obtained. Typical properties of the cured resins are shown in the attached Figure 5 , 6 and 7.

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Abstract

The invention discloses composite expandable flame retardant modified thermosetting resin and a preparation method thereof. The preparation method comprises the following steps of: adding mixed solution of phosphorus oxychloride and dioxane into suspension liquid of expandable graphite and dioxane which are evenly mixed, adding polyol and catalyst, then adding 1, 3, 5-triglycidyl isocyanurate, and after reaction is ended, conducting suction filtration, washing and drying to obtain composite expandable flame retardant which contains phosphorous organic expandable flame retardant which covers the surface of inorganic expandable graphite in a chemical bonding way; and evenly mixing thermosetting resin and the composite expandable flame retardant according to weight ratio of 95:5 to 80:20 at the melting temperature of the resin to obtain the composite expandable flame retardant modified thermosetting resin. On the premise that the modified resin reserves the excellent heat resistance of the thermosetting resin, the modified resin has excellent flame retardant performance. The preparation method provided by the invention has the characteristics of high applicability, simple operation process and high flame retardant performance.

Description

technical field [0001] The invention relates to the technical field of flame-retardant polymer materials, in particular to a composite expansion flame retardant-modified thermosetting resin and a preparation method thereof. Background technique [0002] High-performance thermosetting resins are indispensable and important basic materials in modern industrial fields. However, the flame retardancy of existing high-performance thermosetting resins still cannot meet the requirements for use. Therefore, how to obtain outstanding flame retardancy on the basis of maintaining the excellent properties of existing high-performance thermosetting resins has become a hot spot in the field of material research and development today. [0003] It is a very effective way to improve the flame retardancy of polymer materials by adding flame retardants. Intumescent flame retardant (IFR) is a highly efficient halogen-free flame retardant, which has the advantages of low smoke, low toxicity, lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K7/24C08K3/04C08L79/04C08L63/02C08L79/08
Inventor 梁国正韩纪鹏顾嫒娟袁莉
Owner SUZHOU UNIV
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