CN101985512A - Physically expandable microsphere epoxy foaming material and preparation method thereof - Google Patents

Physically expandable microsphere epoxy foaming material and preparation method thereof Download PDF

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Publication number
CN101985512A
CN101985512A CN2010101123195A CN201010112319A CN101985512A CN 101985512 A CN101985512 A CN 101985512A CN 2010101123195 A CN2010101123195 A CN 2010101123195A CN 201010112319 A CN201010112319 A CN 201010112319A CN 101985512 A CN101985512 A CN 101985512A
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China
Prior art keywords
parts
temperature
epoxy
curing
physics
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CN2010101123195A
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Chinese (zh)
Inventor
罗恒
张纯
秦舒浩
兰新
付军
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National Composite Modified Polymer Material Engineering Technology Research Cen
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National Composite Modified Polymer Material Engineering Technology Research Cen
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Priority to CN2010101123195A priority Critical patent/CN101985512A/en
Publication of CN101985512A publication Critical patent/CN101985512A/en
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Abstract

The invention discloses a physically expandable microsphere epoxy foaming material and a preparation method thereof. The material comprises the following raw materials in parts by weight: 52-100 parts of epoxy resin, 42-80 parts of curing agent, 0.08-0.2 part of promoter, 10-20 parts of reinforcing filler, 8-10 parts of flexibilizer and 1.5-3 parts of foaming microspheres. The preparation method comprises the following steps: mixing the raw materials evenly, placing the mixture in 95-130 DEG C of water bath or oil bath to heat, stirring and heating for a half hour to ensure that the viscosity of the mixture is 3000-3300mPa.s, adding foaming microspheres, stirring for 1-3min, pouring in a fiber glass-reinforced plastic mould; pushing the mould in an electronic microwave heating box to cure and release heat, wherein when the exothermic temperature is 120-135 DEG C, the foaming agent begins to foam and expand and relaizes curing and forming; keeping the temperature to 80-130 DEG C for 0-5 hours, performing post-curing, then reducing the temperature to the room temperature and demoulding. The method of the invention is characterized in that the heating speed is high, the temperature distribution is uniform, the material has no bad foam, and the foams have the same size and are distributed uniformly.

Description

Physics expended microsphere epoxy foam material and production method thereof
Technical field
The present invention relates to the material technology field, relate in particular to a kind of foam material, also relate to its production method simultaneously.
Background technology
Existing epoxy foam material adopts chemical foaming agent to add in the object as the foaming source and material when being heated to a certain temperature jointly, and the chemical foaming agent decomposes produces gas and forms small pore, promptly forms the foam material with small pore after the curing.But whipping agent is stayed in the material after decomposing, and is influential to foam performance, and big smell is arranged when decomposing simultaneously.Be that the mould that material is housed is pushed in the baking oven when it is produced, by adding warm air, warm air heating mould again then, by the material in the heat reheat mould of mould, length consuming time like this heats also inhomogeneously, and the curing of material is also wayward.
Summary of the invention
The object of the present invention is to provide that a kind of rate of heating is fast, temperature is even, noresidue and peculiar smell, anosis bubble is evenly distributed, physics expended microsphere epoxy foam material of the same size.
Another object of the present invention is to provide the production method of this physics expended microsphere epoxy foam material.
Physics expended microsphere epoxy foam material of the present invention, form by the raw material of following weight part:
Resins, epoxy: 52~100 parts
Solidifying agent: 42~80 parts
Promotor: 0.08~0.2 part
Enhancing property stopping composition: 10~20 parts
Toughner: 8~10 parts
Whipping agent: 1.5~3 parts
Above-mentioned physics expended microsphere epoxy foam material, wherein: Resins, epoxy is one or both of bisphenol A epoxide resin, polyethers Resins, epoxy.
Above-mentioned physics expended microsphere epoxy foam material, wherein: solidifying agent is methyl tetrahydro phthalic anhydride or methyl carbic anhydride.
Above-mentioned physics expended microsphere epoxy foam material, wherein: promotor is 2,4,6-three (dimethylamino methyl) phenol, 1,8-diaza-bicyclo (5.4.0) hendecene-7 or tetramethyl-bromo-phosphonium.
Above-mentioned physics expended microsphere epoxy foam material, wherein: enhancing property stopping composition is polynite.
Above-mentioned physics expended microsphere epoxy foam material, wherein: toughner is the liquid nitrile rubber.
Above-mentioned physics expended microsphere epoxy foam material, wherein: whipping agent is a foam microspheres.
The production method of a kind of physics expended microsphere epoxy foam material of the present invention, comprise: after above-mentioned raw materials is stirred, place the water-bath internal heating, water-bath or oil bath temperature are set at 95~130 ℃, and stirring heating half an hour is after reaching 3000~3300mPas, add foam microspheres, stirred 1~3 minute, and poured in the fiber reinforced plastic mold, push the electronic microwave heating container, curing exotherm, when exothermic temperature was 120~135 ℃, whipping agent began foaming and intumescing, curing molding, waste heat is taken away by the hydrologic cycle cooling system on the mould, in temperature is 80~130 ℃ of down insulations 0~5 hour, carries out the after fixing moulding, reduce to room temperature then after the demoulding promptly.
The present invention compared with prior art, has tangible beneficial effect, as can be known from the above technical solutions, the whipping agent that adopts is inflatable physics microballoon, it is to wrap a kind of gas by the elastic capsule of a kind of tool, the gas expansion capsule arrives original tens times after being heated, and this state curing molding is formed epoxy foam material.Stay in the material whipping agent and be made up of the capsule after air porous expanded, size evenly and does not have the smell of decomposition when flexible, foaming; Forming mould and material adopt the electronic microwave heating, directly passing mould heats material, rate of heating is fast, temperature is even, thereby reach the curing that is rapidly heated, the nano level polynite that adds modification improves more than (20%) strength of materials, add the liquid butadiene acrylonitrile rubber and increase toughness (20%), Resins, epoxy, solidifying agent and promotor are stirred curing and are reached certain viscosity, after soon material will be poured in the fiber reinforced plastic mold, adopt the electronic microwave heating to be rapidly heated, it is consistent that the material heat release temperature that the after fixing of resin heat radiation is caused and the temperature of whipping agent foaming are made as, and quoting intensification and reaching the foaming purpose.No chemical residue and whipping agent smell problem, anosis bubble is evenly distributed, size is consistent.
Embodiment
Embodiment 1
A kind of production method of physics expended microsphere epoxy foam material comprises the steps:
(1) take by weighing the raw material of following weight:
Bisphenol A epoxide resin 100 grams
Methyl tetrahydro phthalic anhydride 80 grams
2,4,6-three (dimethylamino methyl) phenol 0.2 gram
Polynite 10 grams
Nitrile rubber 8 grams
Foam microspheres 2.85 grams
(2) above-mentioned raw materials is stirred after, place the water-bath internal heating, bath temperature is set at 95 ℃, stirring heating half an hour, after reaching 3200mPas, add foam microspheres, stirred 3 minutes, pour in the fiber reinforced plastic mold, push the electronic microwave heating container, curing exotherm is when exothermic temperature is 135 ℃, whipping agent begins foaming and intumescing, curing molding, waste heat is taken away by the hydrologic cycle cooling system on the mould, is 110 ℃ in temperature and is incubated 4 hours down, carry out the after fixing moulding, reduce to room temperature then after the demoulding promptly.
Section is through electron microscope observation, and it foams aperture about 100 μ m, uniform distribution; Shock strength 5.07kJ/m 2, flexural strength 39.4MPa, shrinking percentage 0.10%, proportion 0.8g/m 2
Embodiment 2
A kind of production method of physics expended microsphere epoxy foam material comprises the steps:
(1) take by weighing the raw material of following weight:
Bisphenol A epoxide resin 50 grams
Methyl carbic anhydride 45 grams
1,8-diaza-bicyclo (5.4.0) hendecene-70.08 gram
Polynite 15 grams
Nitrile rubber 8 grams
Foam microspheres 1.5 grams.
(2) above-mentioned raw materials is stirred after, place the oil bath internal heating, oil bath temperature is set at 125 ℃, stirring heating half an hour, after reaching 3000mPas, add foam microspheres, stirred 2 minutes, and poured in the fiber reinforced plastic mold, push the electronic microwave heating container, curing exotherm, when exothermic temperature was 130 ℃, whipping agent began foaming and intumescing, the final curing moulding, naturally reduce to room temperature, the demoulding promptly.
Section is through electron microscope observation, and it foams aperture about 100 μ m, uniform distribution; Shock strength 2.67kJ/m 2, flexural strength 30.5MPa, shrinking percentage 0.15%, proportion 0.85g/m 2
Embodiment 3
A kind of production method of physics expended microsphere epoxy foam material comprises the steps:
(1) take by weighing the raw material of following weight:
Polyethers Resins, epoxy 50 grams
High viscosity methyl tetrahydro phthalic anhydride 42 grams
Tetramethyl-bromo-phosphonium 0.09 gram
Polynite 20 grams
Liquid nitrile rubber 10 grams
Foam microspheres 3 grams.
(2) above-mentioned raw materials is stirred after, place the oil bath internal heating, oil bath temperature is set at 130 ℃, stirring heating half an hour, after reaching 3300mPas, add foam microspheres, stirred 1 minute, and poured fiber reinforced plastic mold into, push the electronic microwave heating container, curing exotherm, exothermic temperature are 120 ℃, curing molding, be 130 ℃ in temperature and be incubated 1 hour down, being 100 ℃ of down insulations 2 hours in temperature again, is 80 ℃ of insulations 2 hours down in temperature again, reduce to room temperature then after the demoulding promptly.
Section is through electron microscope observation, and it foams aperture about 100 μ m, uniform distribution; Shock strength 4.0kJ/m 2, flexural strength 38.8MPa, shrinking percentage 1.4%, proportion 0.82g/m 2
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, any technical solution of the present invention content that do not break away from,, all still belong in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.

Claims (3)

1. physics expended microsphere epoxy foam material, form by the raw material of following weight part:
Resins, epoxy: 52~100 parts
Solidifying agent: 42~80 parts
Promotor: 0.08~0.2 part
Enhancing property stopping composition: 10~20 parts
Toughner: 8~10 parts
Whipping agent: 1.5~3 parts
Wherein: Resins, epoxy is one or both of bisphenol A epoxide resin, polyethers Resins, epoxy;
Solidifying agent is methyl tetrahydro phthalic anhydride or methyl carbic anhydride;
Promotor is 2,4,6-three (dimethylamino methyl) phenol, 1,8-diaza-bicyclo (5.4.0) hendecene-7 or tetramethyl-bromo-phosphonium;
Enhancing property stopping composition is polynite;
Toughner is the liquid nitrile rubber;
Whipping agent is a foam microspheres.
2. the production method of a kind of physics expended microsphere epoxy foam material as claimed in claim 1, comprise: after above-mentioned raw materials is stirred, place the water-bath internal heating, water-bath or oil bath temperature are set at 95~130 ℃, stirring heating half an hour, after reaching 3000~3300mPas, add foam microspheres, stirred 1~3 minute, pour in the fiber reinforced plastic mold, push the electronic microwave heating container, curing exotherm, when exothermic temperature is 120~135 ℃, whipping agent begins foaming and intumescing, and curing molding is 80~130 ℃ in temperature and is incubated 0~5 hour down, carry out the after fixing moulding, reduce to room temperature then after the demoulding promptly.
3. the production method of a kind of physics expended microsphere epoxy foam material as claimed in claim 2, wherein: the waste heat behind the curing exotherm is taken away by the hydrologic cycle cooling system on the mould.
CN2010101123195A 2010-02-23 2010-02-23 Physically expandable microsphere epoxy foaming material and preparation method thereof Pending CN101985512A (en)

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Application Number Priority Date Filing Date Title
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CN101985512A true CN101985512A (en) 2011-03-16

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104861424A (en) * 2015-06-05 2015-08-26 武汉理工大学 Preparation method of polymer-based light high-strength foam material
CN105647127A (en) * 2014-12-05 2016-06-08 贵州航天天马机电科技有限公司 Epoxy foam flame-retardant material and preparation method thereof
CN106414640A (en) * 2015-04-10 2017-02-15 株式会社寺冈制作所 Adhesive sheet
CN106633634A (en) * 2016-10-26 2017-05-10 四川大学 Epoxy resin foam material containing perforated structure and preparation method thereof
CN106674894A (en) * 2016-12-06 2017-05-17 云南光电辅料有限公司 Epoxy composite material and decomposition recovery method thereof
CN107108379A (en) * 2014-12-11 2017-08-29 建筑研究和技术有限公司 The method of cement of the manufacture comprising expanded polymeric microspheres
CN107501599A (en) * 2017-08-15 2017-12-22 成都新柯力化工科技有限公司 A kind of whisker by expandable microspheres foaming supports polypropylene plastics and preparation method
CN109792075A (en) * 2016-08-05 2019-05-21 阿姆泰克研究国际公司 Composite porous and relevant device, method and the purposes of cured, suitable type

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105647127A (en) * 2014-12-05 2016-06-08 贵州航天天马机电科技有限公司 Epoxy foam flame-retardant material and preparation method thereof
CN107108379A (en) * 2014-12-11 2017-08-29 建筑研究和技术有限公司 The method of cement of the manufacture comprising expanded polymeric microspheres
CN106414640A (en) * 2015-04-10 2017-02-15 株式会社寺冈制作所 Adhesive sheet
CN108410376A (en) * 2015-04-10 2018-08-17 株式会社寺冈制作所 Adhesive sheet
TWI711681B (en) * 2015-04-10 2020-12-01 日商寺岡製作所股份有限公司 Adhesive sheet
TWI792081B (en) * 2015-04-10 2023-02-11 日商寺岡製作所股份有限公司 Adhesive sheet
CN104861424A (en) * 2015-06-05 2015-08-26 武汉理工大学 Preparation method of polymer-based light high-strength foam material
CN109792075A (en) * 2016-08-05 2019-05-21 阿姆泰克研究国际公司 Composite porous and relevant device, method and the purposes of cured, suitable type
CN106633634A (en) * 2016-10-26 2017-05-10 四川大学 Epoxy resin foam material containing perforated structure and preparation method thereof
CN106674894A (en) * 2016-12-06 2017-05-17 云南光电辅料有限公司 Epoxy composite material and decomposition recovery method thereof
CN107501599A (en) * 2017-08-15 2017-12-22 成都新柯力化工科技有限公司 A kind of whisker by expandable microspheres foaming supports polypropylene plastics and preparation method

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Open date: 20110316