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Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic

A technology of rigid polyurethane and expanded graphite, applied in the field of flame retardant polyurethane foam, can solve the problems of decreased mechanical properties of foam, decreased flame retardant effect, increased thermal conductivity, etc. performance effect

Inactive Publication Date: 2014-02-05
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through research, it is found that the flame retardant effect of expandable graphite in rigid polyurethane foam is closely related to its particle size. The larger the particle size, the better the flame retardant effect, but it leads to a decrease in the mechanical properties of the foam and an increase in thermal conductivity; When the particle size of expandable graphite is small, although the influence on the mechanical properties and thermal conductivity of the foam is reduced, its flame retardant effect is also significantly reduced
In addition, the addition of expandable graphite inevitably leads to the destruction of the polyurethane rigid foam cell structure, which makes the products generally have the problem of increased thermal conductivity.

Method used

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  • Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic
  • Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic
  • Core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and application thereof in rigid polyurethane foaming plastic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Preparation of core-shell synergistic polyurethane microencapsulated expandable graphite: In a 500ml four-neck flask equipped with a thermometer, a mechanical stirrer and a reflux condenser, add 10g of β-cyclodextrin (β-CD) and 50ml of dimethyl sulfoxide (DMSO), stirring and raising the temperature to 80 ° C, after the cyclodextrin is completely dissolved, add 10 g of toluene diisocyanate (TDI) and 50 ml, 4-dioxane, stir at this temperature for 15 to 25 min, then Add 100g of expandable graphite particles (400 mesh), 200ml of 1,4-dioxane, 2g of OP-10 and 0.4g of dibutyltin dilaurate (DBTDL), and heat up to 85°C for 2 hours. Cool to room temperature, filter, wash with water and dry to obtain core-shell synergistic polyurethane microencapsulated expandable graphite PUEG-1.

[0063] Preparation of halogen-free flame-retardant rigid polyurethane foam: 40g of polyether polyol 635 (hydroxyl value 498mg KOH / g), 60g of aromatic polyester polyol (hydroxyl value 412mg KOH / g), 10g ...

Embodiment 2

[0066] Preparation of core-shell synergistic polyurethane microencapsulated expandable graphite: In a 500ml four-neck flask equipped with a thermometer, a mechanical stirrer and a reflux condenser, add 20g of β-cyclodextrin (β-CD) and 70ml DMSO, Stir and heat up to 80°C. After the cyclodextrin is completely dissolved, add 20g of toluene diisocyanate (TDI) and 70ml of l,4-dioxane, stir at this temperature for 15-25min, and add 100g of expandable Graphite particles (400 mesh), 200ml l,4-dioxane, 2g OP-10 and 0.4g dibutyltin dilaurate (DBTDL), heated up to 85°C for 2h. Cool to room temperature, filter, wash with water and dry to obtain core-shell synergistic polyurethane microencapsulated expandable graphite PUEG-2.

[0067]Preparation of halogen-free flame-retardant rigid polyurethane foam: 40g of polyether polyol 4110 (hydroxyl value 420mg KOH / g), 60g of phthalic anhydride polyester polyol (hydroxyl value 240mg KOH / g), 10g of microcapsules Expandable graphite PUEG-2, 5g of die...

Embodiment 3

[0070] Preparation of halogen-free flame-retardant rigid polyurethane foam: 40 g of polyether polyol 4110 (hydroxyl value 420 mg KOH / g), 60 g of rosin polyester polyol (hydroxyl value 360 ​​mg KOH / g), 10 g of microcapsules Thin expandable graphite PUEG-2 (with embodiment 2), the diethyl ethyl phosphonate (DEEP) of 5g, the melamine polyphosphate (MPP) of 5g, the nickel-aluminum metal double hydroxide of the organic modification of 1.5g (Ni-Al-OLDH, self-made, preparation method sees embodiment 2 references for details), the pentane of 20g, the foam stabilizer (JSY-5081) of 5g, after the tetramethylpropanediamine of 0.5g mixes, with maximum After stirring at a rotating speed for 1min, mix it with 120g of crude MDI, stir at room temperature for 20s at the maximum stirring rate, and quickly pour it into a preheated rigid foam mold for pressure foaming to obtain a halogen-free flame-retardant rigid polyurethane foam .

[0071] The above-mentioned halogen-free flame-retardant rigid...

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Abstract

The invention discloses a core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite and the application of the expandable graphite in rigid polyurethane foaming plastic. The core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite comprises polyether and / or polyester polyol, a foaming agent, a foam stabilizer, a catalyst, an organic phosphorus-based flame retardant, a halogen-free intumescent flame retardant, an organic modified nano inorganic filler, core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite, polyisocyanate compound and isocyanate index, wherein the polyisocyanate compound has two or more isocyanate groups; the core-shell synergistic flame retardant polyurethane microencapsulation expandable graphite takes expandable graphite particles as a capsule core and takes cyclodextrin or polyurethane as a capsule shell, wherein the cyclodextrin or polyurethane is formed by crosslinking cyclodextrin / modified resin and toluene diisocynate. The expandable graphite microcapsule can effectively improve the initial decomposition temperature, the heat stability and the flame retardant effect of a material and remarkably reduces the heat release rate and the total heat release quality during combustion.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polyurethane foam, in particular to a core-shell synergistic flame-retardant polyurethane microencapsulated expandable graphite and its application in rigid polyurethane foam. Background technique [0002] Rigid polyurethane foam has the advantages of low density, high strength, low thermal conductivity, strong adhesion, and convenient construction. It can be used as thermal insulation materials and structural load-bearing materials, and is widely used in construction, transportation, refrigerators, freezers, petroleum Chemical pipelines, aviation military and other fields. However, due to the large specific surface area, low density and low thermal conductivity of the foam itself, the oxygen index of rigid polyurethane without flame retardant treatment is lower than 19%, which is a flammable material and emits toxic gases such as HCN and CO during combustion. , often bring serious harm t...

Claims

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Application Information

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IPC IPC(8): C08G18/76C08G18/48C08G18/42C08K13/06C08K9/04C08K3/34C08K3/32C08K5/5333C08K3/22C08K5/55C08K5/3492C08K5/523C08K7/00C08J9/14C08L75/06C08L75/08B01J13/18C08G18/64C08G18/62C08K9/00C08K3/04C08L75/04C08G101/00
CPCC08G18/4018C08G18/6484C08J9/141C08J9/144C08J2203/14C08J2203/142C08J2375/06C08J2375/08C08K3/04C08K3/346C08K7/24C08K9/04C08K9/10C08K13/06C08G2110/0025C08G2110/0075
Inventor 高丽萍郑光耀
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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