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A kind of preparation method of reinforced and toughened flame-retardant phenolic foam

A phenolic foam, strengthening and toughening technology, applied in the field of materials, can solve the problems of reduced flame retardant performance, high hardness and property loss of phenolic foam, and achieve the effect of excellent flame retardant performance

Active Publication Date: 2017-05-31
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, they are very flammable materials that can easily catch fire and cause fire accidents, causing significant casualties and property damage
Although phenolic foam has the advantages of excellent flame retardancy, good flame penetration resistance, low smoke and low toxicity when burning, but phenolic foam also has the defects of high brittleness, high hardness and easy pulverization, which seriously limits the application of phenolic foam. Therefore, it is necessary to toughen the phenolic foam
[0003] According to literature reports [Plastic Industry, 2011, 39(2): 25-27; FRP / composite materials, 2011, (2): 37-39; China Plastics, 2005, 19(12): 53-56; Henan Chemical Industry, 2006, 23(9): 22-23; Applied Chemical Industry, 2010, 39(11), 1693-1695.], polymer tougheners commonly used in phenolic foam, such as liquid nitrile rubber, polyurethane prepolymer, polyacrylic acid Although n-butyl ester, flexible epoxy resin, polyethylene glycol, etc. are flammable, they can improve the toughness of phenolic foam, but usually reduce the flame retardancy of phenolic foam
When fiber (such as short glass fiber) is used as a toughening agent, the viscosity of the resin will be greatly increased, and the mixing process will become difficult. At the same time, the fiber will be oriented along the flow direction of the resin and affect the formation of foam, reducing the quality of foam and foam. Uniformity, this method is difficult to meet the actual use requirements [J. Appl. Polym. Sci.2007, 104(3), 1399-1407]

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 80g of PEG400 into a three-neck bottle, stir vigorously at 50°C, add 7.1g of phosphorus pentoxide into it in 5 batches, and after the particles are basically dissolved, raise the temperature to 70°C and keep it for 1.5 hours, then continue to heat up to 110°C ℃ for 4 hours; 2.1 g of boric acid was added at one time, and reacted at 110 ℃ for 3 hours to obtain dark yellow viscous flame retardant toughening agent 1.

[0022] Weigh 100 parts of resole phenolic resin, respectively mix 5 parts of surfactant, 5 parts of flame retardant and toughening agent 1, 5 parts of nano-alumina dispersion, 9 parts of mixed acid curing agent (water: toluene-4-sulfonic acid: Phosphoric acid = 2:2:1) and 8 parts of physical foaming agent were added to it, stirred evenly, poured into the mold, and foamed at 80°C for 1 hour to obtain a phenolic foam with no halogen, flame retardancy, strengthening and toughening, and low pulverization rate plastic.

Embodiment 2

[0024] Weigh 40g of PEG200 into a three-neck bottle, stir vigorously at 60°C, add 4.7g of phosphorus pentoxide into it in 3 batches, and after the particles are basically dissolved, raise the temperature to 80°C and keep it for 1 hour, then continue to heat up to 120°C ℃ for 5 hours; add 4.2 g of boric acid at one time, and react at 120 ℃ for 2 hours to obtain yellow viscous flame retardant toughening agent 2.

[0025] Weigh 100 parts of resole phenolic resin, respectively mix 5 parts of surfactant, 5 parts of flame retardant and toughening agent 2, 5 parts of nano-zirconia dispersion, 9 parts of mixed acid curing agent (water: toluene-4-sulfonic acid: Phosphoric acid = 2:2:1) and 8 parts of physical foaming agent were added to it, stirred evenly, poured into the mold, and foamed at 80°C for 1 hour to obtain a phenolic foam with no halogen, flame retardancy, strengthening and toughening, and low pulverization rate plastic).

Embodiment 3

[0027] Weigh 120g of PEG600 into a three-neck bottle, stir vigorously at 40°C, add 2.4g of phosphorus pentoxide into it in 2 batches, and after the particles are basically dissolved, raise the temperature to 60°C and keep it for 1.5 hours, then continue to heat up to 130°C ℃ for 6 hours; add 6.3 g of boric acid at one time, and react at 110 ℃ for 3 hours to obtain light yellow viscous flame retardant toughener 3.

[0028] Weigh 100 parts of resole phenolic resin, respectively mix 5 parts of surfactant, 5 parts of flame retardant and toughening agent 3, 5 parts of nano-magnesium oxide dispersion, 9 parts of mixed acid curing agent (water: toluene-4-sulfonic acid: Phosphoric acid = 2:2:1) and 8 parts of physical foaming agent were added to it, stirred evenly, poured into the mold, and foamed at 80°C for 1 hour to obtain a phenolic foam with no halogen, flame retardancy, strengthening and toughening, and low pulverization rate plastic.

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PUM

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Abstract

The invention relates to a preparation method for reinforced and toughened flame-retardant phenolic foam. The preparation method comprises: adding polyethylene glycol into a three-necked bottle, adding phosphorus pentoxide in batches under quick stirring at 30-60 DEG C, and after phosphorus pentoxide is almost dissolved, raising the temperature to 65-85 DEG C and maintaining the temperature for 1-3 hours, and then raising the temperature to 100-140 DEG C for reaction for 3-6 hours; and adding boric acid by one time and maintaining the temperature at 100-140 DEG C for 2-4 hours to obtain a faint yellow to deep yellow product, namely a polyethylene glycol borate phosphate flame-retardant flexibilizer, wherein the molar ratio of hydroxyl groups in polyethylene glycol to total acid hydroxyl groups in phosphorus pentoxide and boric acid is 1:1 to 1:3; the preparation method for the reinforced and toughened flame-retardant phenolic foam comprises: firstly weighing 100 parts of stage A phenolic resin; then separately adding a borate flame-retardant modifier, a surfactant, a curing agent and a foaming agent; quickly and uniformly stirring the mixture; adding the mixture into a die and closing the die; and carrying out foaming curing at 70-90 DEG C for 40-80 minutes to obtain the reinforced and toughened flame-retardant phenolic foam.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for preparing a reinforced and toughened flame-retardant phenolic foam compounded with a flame-retardant toughening agent and nano oxides. Background technique [0002] Currently commonly used polymer foam materials, such as polystyrene foam and polyurethane foam, are widely used due to their excellent thermal insulation performance, good mechanical properties and easy molding and processing. However, they are very flammable materials, which can easily catch fire and cause fire accidents, causing heavy casualties and property losses. Although phenolic foam has the advantages of excellent flame retardancy, good flame penetration resistance, low smoke and low toxicity when burning, but phenolic foam also has the defects of high brittleness, high hardness and easy pulverization, which seriously limits the application of phenolic foam. Therefore, it is very ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/06C08L71/02C08K3/22C08J9/14C08G65/327C08G65/328
Inventor 王正洲朱羽翔李晓艳
Owner TONGJI UNIV