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Preparation method of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane/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, can solve the flame-retardant and fire-resistant properties of epoxy resin Insufficient, cumbersome and difficult preparation steps of flame retardant epoxy resin, etc., to achieve excellent flame retardant and fire resistance, improved mechanical properties, and increased stability

Active Publication Date: 2015-08-19
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the shortcoming of this preparation method is that the flame retardant and fire resistance of the prepared epoxy resin is insufficient, even if the flame retardant addition is 15% by weight, the highest oxygen index can only reach 31%
Chinese Patent Publication No. CN101343403A provides a halogen-free flame retardant epoxy resin composition, which contains phosphorus epoxy resin, curing agent, toughening agent and solvent, although the environmental protection is significantly improved by blending with polyamide resin The adhesion and flexibility of the epoxy resin composition are at the expense of the flame retardant properties of the material itself, and it also makes the preparation steps of the flame retardant epoxy resin cumbersome and difficult.

Method used

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  • Preparation method of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane/epoxy resin hybrid material
  • Preparation method of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane/epoxy resin hybrid material
  • Preparation method of phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane/epoxy resin hybrid material

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Experimental program
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Effect test

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 dried product 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 After st...

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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Abstract

The invention discloses a preparation method of a phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane / epoxy resin hybrid material, which comprises the following steps: in the presence of a solvent and an initiator, carrying out free-radical polymerization on glycidyl methacrylate, phosphorus-containing monomer and acryloyloxypropyl heptaisobutyl POSS (polyhedral oligomeric silsesquioxane) to obtain a phosphorus-containing POSS-base compound, uniformly mixing an epoxy resin and the phosphorus-containing POSS-base compound at certain temperature, adding a curing agent, evenly mixing, pouring into a mold, and removing bubbles in vacuum; and finally, curing, and demolding to obtain the phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane / epoxy resin hybrid material. The phosphorus-containing flame-retardant POSS / epoxy resin hybrid material is free of halogen, has the advantages of no toxic or side effect, simple technique, favorable flame retardancy, low manufacturing cost and high transparency, and can be widely used in the fields of manufacturing of optical components, LED (light-emitting diode) packaging and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a method for preparing a phosphorus-containing flame-retardant organic-inorganic hybrid silsesquioxane and epoxy resin hybrid material. Background technique [0002] Cured epoxy resin is widely used in the bonding, packaging and printing of electronic components because of its good thermal stability, insulation, adhesiveness, good mechanical properties and molding process performance, and relatively low cost. The substrate processing of circuit board (PCB) is one of the important electronic materials. [0003] Generally, the cured epoxy resin is flammable, and there is a fire hazard during use. So far, in the electrical and electronic field, bromine flame-retardant epoxy resins are mainly used. However, brominated epoxy-based electronic materials will release toxic substances such as irritating strong acid gases and strong carcinogens such as polybrominated dibenzofurans during...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/02C08L43/02C08L43/04C08L33/14C08F230/02C08F230/08C08F220/28
Inventor 戴李宗陈国荣吴顺伟刘诚罗伟昂许一婷曹莹项嘉懿曾碧榕
Owner XIAMEN UNIV
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