Preparation method of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane and epoxy resin hybrid material
A technology of silsesquioxane and epoxy resin, which is applied in the field of preparation of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane and epoxy resin hybrid materials, and can solve the preparation steps of flame-retardant epoxy resin Complicated, difficult, insufficient flame retardant and fire-resistant properties of epoxy resin, etc., to achieve excellent flame retardant and fire resistance, increase stability, and improve mechanical properties
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Embodiment 1
[0027] 1) Preparation of phosphorus-containing POSS-based compounds: In a 1000mL reaction vessel, 26g of glycidyl methacrylate, 132g of phosphorus-containing monomers, 41g of AiBuPOSS (acryloxypropyl heptaisobutyl cage silsesquioxane alkane) and 1g of initiator azobisisobutyronitrile (AIBN) were dissolved in 500mL of tetrahydrofuran, stirred and reacted for 24h at 65°C under the protection of nitrogen; after the reaction, the reaction solution was purified by precipitation with methanol, and the dried product was a yellow powder. It is a phosphorus-containing POSS-based compound, and the molecular structure of the phosphorus-containing POSS-based compound is shown in formula (I):
[0028]
[0029] Wherein x:y:z=1:1:8, relative molecular weight is 27824;
[0030] The molecular structural formula of the phosphorus-containing monomer is shown in formula (II), and its preparation method refers to Chinese patent CN104262398A;
[0031]
[0032] 2) Preparation of phosphorus-co...
Embodiment 2
[0034] 1) Preparation of phosphorus-containing POSS-based compounds: In a 1000mL reaction vessel, 26g of glycidyl methacrylate, 132g of phosphorus-containing monomer, 46g of AiBuPOSS and 1g of initiator AIBN were dissolved in 500mL of tetrahydrofuran. Under protection, the reaction was stirred for 24 hours; after the reaction, the reaction solution was purified by precipitation with methanol, and the product after drying was a yellow powder, which was a phosphorus-containing POSS-based compound. The molecular structure of the phosphorus-containing POSS-based compound was shown in formula (I):
[0035]
[0036] Wherein x:y:z=1:1:7, relative molecular weight is 34638;
[0037] Described phosphorus-containing monomer is with embodiment 1;
[0038]2) Preparation of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane and epoxy resin hybrid material: 100g of epoxy resin (E-51) and 10g of phosphorus-containing POSS-based compound obtained in step 1) in A...
Embodiment 3
[0040] 1) Preparation of phosphorus-containing POSS-based compounds: In a 1000mL reaction vessel, 26g of glycidyl methacrylate, 127g of phosphorus-containing monomer, 46g of AiBuPOSS and 1g of initiator AIBN were dissolved in 500mL of tetrahydrofuran. Under protection, the reaction was stirred for 24 hours; after the reaction, the reaction solution was purified by precipitation with methanol, and the product after drying was a yellow powder, which was a phosphorus-containing POSS-based compound. The molecular structure of the phosphorus-containing POSS-based compound was shown in formula (I):
[0041]
[0042] Wherein x:y:z=1:1:6, relative molecular weight is 37824;
[0043] Described phosphorus-containing monomer is with embodiment 1;
[0044] 2) Preparation of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane and epoxy resin hybrid material: 100g of epoxy resin (E-51) and 15g of phosphorus-containing POSS-based compound obtained in step 1) in ...
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