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Compound intumescent flame retardant and preparation method thereof

An intumescent flame retardant and composite technology, applied in the field of intumescent flame retardants and their preparation, can solve the problems of difficult dispersibility and interfacial force, deteriorating physical and mechanical properties, affecting flame retardant properties, etc., and achieve excellent thermal oxygen shielding. effect, good flame retardant effect, thermal and mechanical properties improvement effect

Inactive Publication Date: 2014-01-01
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Secondly, 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 and may deteriorate other physical and mechanical properties
Third, in order to obtain the flame retardant effect of chemical intumescent flame retardants, generally chemical intumescent flame retardants need to be added in a higher amount (see literature: Gao F, Tong LF, Fang ZP. Effect of a novel phosphorous–nitrogen containing intumescent flame retardant on the fire retardancy and the thermal behavior of poly(butylene terephthalate). Polymer Degradation and Stability. 2006;91:1295-9.), which reduces the heat resistance of the material

Method used

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  • Compound intumescent flame retardant and preparation method thereof
  • Compound intumescent flame retardant and preparation method thereof
  • Compound intumescent flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 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;

[0027] 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;

[0028] 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 reaction solution In E, the temperature was raised to 80° C. for ...

Embodiment 2

[0040] 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;

[0041] 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;

[0042] 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 reaction solution In E, the temperature was raised to 90°C for 1...

Embodiment 3

[0045] Add 5g of 320 mesh expandable graphite and 60g of dioxane into a three-necked flask, stir and mix evenly to obtain a suspension A of expandable graphite;

[0046] Add 1.85g of phosphorus oxychloride to 18.5g 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 for 2 hours under nitrogen protection to obtain reaction solution D in which phosphoryl chloride-formed expandable graphite is formed;

[0047] According to the molar ratio of phosphorus oxychloride and pentaerythritol as 1:1, 1.64g of pentaerythritol was added to the above reaction solution D, and 0.0033g of anhydrous stannous chloride was added; the temperature was raised to 60°C for 2 hours to obtain reaction solution E. According to the pentaerythritol and 1,3,5-triglycidyl-S-triazinetrione molar ratio of 1:2, 7.17g of 1,3,5-triglycidyl-S-triazinetrione was added to the reaction solution In E, the temperature was raised to 80° ...

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Abstract

The invention relates to a compound intumescent flame retardant and a preparation method thereof. The method comprises the following steps of: adding a mixed solution of phosphorus oxychloride and dioxane into a suspension obtained by uniformly mixing expandable graphite with dioxane, and reacting in a nitrogen atmosphere at 40-60 DEG C for 0.5-2 hours; adding polyalcohol and a catalyst, and reacting at 50-70 DEG C for 3-5 hours; and adding 1,3,5-triepihydric alcohol-S-triazinetrione, reacting at 80-100 DEG C for 8-15 hours, leaching, washing and drying to obtain a compound intumescent flame retardant in which a phosphorus-containing organic intumescent flame retardant is coated on the surface of inorganic phase expandable graphite in a chemical bonding way. During combustion, a denser protective layer can be formed, so that an excellent thermal oxidation shielding effect is achieved; and the compound intumescent flame retardant contains a large quantity of hydroxyl radicals and epoxy groups, so that high interface bonding force and high dispersivity with a high polymer are ensured, and a good flame-retarding effect can be achieved at a low content.

Description

technical field [0001] The invention relates to an intumescent flame retardant and its preparation technology, in particular to an intumescent flame retardant with an organic-inorganic composite structure and a preparation method thereof. Background technique [0002] With the wide application of polymers, their flammability has brought more and more potential hazards to people's lives and properties. How to obtain excellent flame retardancy has become an important topic in polymer research. It is a very effective way to improve the flame retardancy of polymer materials by adding flame retardants. Therefore, the research and development of flame retardants with excellent flame retardancy has become the focus of research. [0003] Intumescent flame retardant (IFR) is a kind of high-efficiency halogen-free flame retardant, which has the advantages of low smoke, low toxicity, low corrosion and no molten dripping during combustion, and has attracted widespread attention. Intume...

Claims

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Application Information

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