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Zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant and preparation method thereof

The technology of a heteropoly acid and a smoke suppressant is applied in the field of zinc-containing Anderson type heteropoly acid flame retardant and smoke suppressant and its preparation, which can solve the problem that the polyoxometalate has poor compatibility with a substrate and a single organic modification method. , low flame retardant efficiency and other problems, to achieve the effect of comprehensive performance improvement, high catalytic activity, high thermal stability

Active Publication Date: 2022-08-09
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to overcome the defects of the prior art and provide a zinc-containing Anderson type heteropolyacid flame retardant and smoke suppressant, which has excellent flame retardant performance and is compatible with the matrix. Good compatibility, which can improve the defects of poor compatibility between polyoxometalates and the matrix, low flame retardant efficiency when used alone, and single and difficult organic modification methods

Method used

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  • Zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant and preparation method thereof
  • Zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant and preparation method thereof
  • Zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0028] (1) Preparation of 2-methoxy-1,3,2λ5-dioxaphosphalane 2-oxide polymerized monomer: under a nitrogen atmosphere, add a 1000 mL condensing reflux tube and a magnetic stirring bar to a In the three-necked flask, add reactants methanol (0.302mol), triethylamine (0.302mol) and 600mL tetrahydrofuran solution, 2-chloro-2-oxygen-1,2,3-dioxaphosphalane (0.302mol) It was diluted with 85 mL of tetrahydrofuran solution and added dropwise to the mixed solution at 0°C. The reaction mixture was stored at -20°C without stirring for 6h. After the reaction was completed, the reaction mixture was filtered with tetrahydrofuran and triethylamine to remove salts. The yellow solution obtained by filtration was subjected to rotary evaporation to form a concentrated solution, which was then washed with CaH 2 The extraction solution is subjected to vacuum distillation to finally form 2-methoxy-1,3,2λ5-dioxaphosphalane 2-oxide, and the specific structural formula is:

[0029]

[0030](2) Pr...

Embodiment 2

[0036] (1) Preparation of 2-isopropoxy-2-oxo-1,3,2-dioxaphosphalane 2-oxide polymerized monomer: under nitrogen atmosphere, to a room equipped with a condenser reflux tube and Add reactant triethylamine (71.9mmol), isopropanol (131mmol) and 100mL of tetrahydrofuran solution, 2-chloro-2-oxygen-1,2,3-dioxaphos-pentane to the three-necked flask of magnetic stirring bar (66.8 mmol) was diluted with 40 mL of tetrahydrofuran, and slowly added dropwise to the mixed solution at -78°C for 1 h. The reaction mixture was stirred at -78°C for 11 h and at 25°C for 9 h. After the reaction was completed, the reaction mixture was filtered with tetrahydrofuran and triethylamine to remove salts. After the yellow solution obtained by filtration was turned into a concentrated solution by rotary evaporation, it was washed with CaH 2 The extraction solution is subjected to vacuum distillation to finally form a colorless oily product 2-isopropoxy-2-oxo-1,3,2-dioxaphosphalane 2-oxide, the specific s...

Embodiment 3

[0044] (1) Preparation of 2-ethoxy-2-oxo-1,3,2-dioxaphosphalane 2-oxide polymerized monomer: under a nitrogen atmosphere, a condensing reflux tube and a magnetic In the 500mL three-necked flask of the stirring bar, the reactants triethylamine (52.4mmol), ethanol (65.2mmol) and 200mL of tetrahydrofuran solution, 2-chloro-2-oxygen-1,2,3-dioxaphosphalane ( 43.5 mmol) was diluted with 70 mL of tetrahydrofuran, and slowly added dropwise to the mixed solution at -78 °C for 5 h. The reaction mixture was stirred at -68°C for 2h and at 25°C for 13h. After the reaction was completed, the reaction mixture was filtered with tetrahydrofuran to remove salts. After the yellow solution obtained by filtration is rotated to form a concentrated solution, the solution is extracted with CaH2 and subjected to vacuum distillation to finally form a colorless oily product 2-ethoxy-2-oxo-1,3,2-dioxo Phosphalane 2-oxide, the specific structural formula is:

[0045]

[0046] (2) Preparation of PPEs...

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Abstract

The invention discloses a zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant and a preparation method thereof. The zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant is prepared by reacting raw materials including succinic anhydride, a polymer PPEs, O-benzotriazole-tetramethylurea hexafluorophosphate, [N (C4H9) 4] 2 [H2ZnMo6O18 {(OCH2) 3CNH2} 2] and triethylamine. The preparation method comprises the following steps: in the presence of succinic anhydride and a dehydrating agent, carrying out ring-opening polymerization reaction on bilateral asymmetrically modified Anerson type polyoxometallate of which the central heteroatom is Zn and monofunctional PPES to obtain a novel zinc-containing Anderson type heteropolyacid flame-retardant smoke suppressant; the difference of POMs and a macromolecular chain in the aspects of charge effect, polarity effect and volume effect is utilized to drive self-aggregation of POMs hybrid molecules in an epoxy matrix to form a nanoscale microscopic phase state or topological structure, so that the purpose of nano synergy is achieved, the comprehensive properties such as flame retardance, mechanical property, heat resistance and dielectric property of the epoxy resin are expected to be improved, and the application prospect is wide. And the special requirements in the high-end manufacturing field of electronic packaging materials and the like are met.

Description

technical field [0001] The invention relates to the field of organic-inorganic hybrid flame retardants, in particular to a zinc-containing Anderson type heteropoly acid flame retardant and smoke suppressant and a preparation method thereof. Background technique [0002] Epoxy resin (EP), as an important thermosetting polymer material, has a wide range of applications and is often used in civil construction due to its advantages of good processability, high reactivity, good mechanical properties, and good electrical insulation. , electronic appliances, aerospace, automotive machinery and so on. However, epoxy resin is flammable, and will produce a large amount of black smoke during the combustion process, which will cause great harm to human life and property, which greatly limits its high requirements for flame retardant standards in electronics, electricity, etc. applications in the field. Therefore, improving the flame retardancy of epoxy resins has become an urgent prob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08L63/02C08L85/02
CPCC08G79/04C08L63/00C08L2201/02C08L2201/08C08L2203/206C08L85/02Y02E60/10
Inventor 陈国荣徐慧戴李宗何思源缪仲熙易新丹罗伟昂许一婷袁丛辉曾碧榕
Owner XIAMEN UNIV
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