CN107033734A - One kind can ceramic epoxy resin fireproof coating - Google Patents
One kind can ceramic epoxy resin fireproof coating Download PDFInfo
- Publication number
- CN107033734A CN107033734A CN201710225388.9A CN201710225388A CN107033734A CN 107033734 A CN107033734 A CN 107033734A CN 201710225388 A CN201710225388 A CN 201710225388A CN 107033734 A CN107033734 A CN 107033734A
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- Prior art keywords
- fireproof coating
- spacing
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- epoxy resin
- stirring
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- Granted
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 83
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 83
- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000000919 ceramic Substances 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims description 59
- 238000003756 stirring Methods 0.000 claims description 45
- 239000000945 filler Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 14
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 10
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 10
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- 239000010445 mica Substances 0.000 claims description 9
- 229910052618 mica group Inorganic materials 0.000 claims description 9
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 9
- 239000010456 wollastonite Substances 0.000 claims description 9
- 229910052882 wollastonite Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 230000002265 prevention Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims 2
- 238000009775 high-speed stirring Methods 0.000 claims 1
- 238000010422 painting Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 238000010073 coating (rubber) Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
- 238000002679 ablation Methods 0.000 description 17
- 238000001291 vacuum drying Methods 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000004079 fireproofing Methods 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000009970 fire resistant effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 229920006334 epoxy coating Polymers 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 244000189799 Asimina triloba Species 0.000 description 1
- 235000006264 Asimina triloba Nutrition 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000009467 Carica papaya Nutrition 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000006182 dimethyl benzyl group Chemical group 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to it is a kind of can ceramic epoxy resin fireproof coating, include nano-silicon dioxide modified epoxy resin preparing the fireproof coating raw material.Due to the addition of nano silicon in the raw material of fireproof coating of the present invention, ceramic can be achieved during burning, preferably, compared to common fireproof silicon/rubber coating system, mechanical property is also higher for the dimensional stability before and after burning.It is more environmentally-friendly and the coating of the present invention is free of volatile organic content, also have great importance for studying economical and practical and high performance fireproof coating.
Description
Technical field
The invention belongs to Flameproof composite material technical field, be related to one kind can ceramic epoxy resin fireproof coating and its
Preparation method.
Background technology
Epoxy resin has excellent adhesive property, mechanical property, corrosion-resistant and heat resistance, it can as coating,
Adhesive and moulding material, are widely used in Aero-Space, electric, engineering technology, civil construction and stationery sports goods system
The field such as make.Wherein, the application of coating ranks first, for example:Body of a motor car priming paint, bridge anticorrosive coating, cement water storage Pot Lining,
Terrace lining is applied, application etc. in ships freight house.But, the security of the lives and property that the inflammability of epoxy resin also gives people brings pole
Big hidden danger, therefore prepare development of the fire-type epoxy coating to national economy and have vital effect.
Anti-flammability refers under the conditions of defined, removes after burning things which may cause a fire disaster, and flame in sample, which is postponed, to be spread and self-extinguish
Characteristic.Common fire retardant mainly include machine system (using bromine system, nitrogen system and red phosphorus and its compound as representative) and it is inorganic system (with
Antimony oxide, magnesium hydroxide, aluminium hydroxide and silicon systems be representative) etc. fire retardant system.But, it is fire-retardant under long duration of action
Material not necessarily fire resisting, and the general all resistance to combustion of refractory material.Fire resistance refers to that under flame or high temperature action material keeps steady
Fixed, the heat-insulated ability with integrality.In general, fire proofing material can expand, foam and carbonize after meeting fire, be formed nonflammable
Spongy carbon layer, and deposit, be covered in external surface layer, the protective effect such as choke, heat-insulated is played to internal material.Therefore, will
Fire proofing material is painted on substrate surface, forms fire resistant coating, can delay the ignition time of base material, the generation of fire preventing, and hinder
Only the intensity of a fire persistently spreads;Or increase thermal insulation is to postpone the time to rupture of matrix structure, be personnel escape, rescue people, fire extinguishing etc.
Play a part of delay, protection, while having the defencive functions such as anti-corrosion, antirust and decoration functions concurrently again.
Current fire proofing material must take into account the requirement of fire-retardant and environmentally friendly two aspects, in low cigarette, low toxicity, non-halogen hair
Exhibition trend.Can ceramic polymer composite using environmental protection, nontoxic, free of contamination material as raw material, at normal temperatures,
It can keep the good elasticity and mechanical property of polymeric matrix;And when running into naked light or in hot environment, and can turn
It is changed into the hard ceramic body with self-supporting, preferably keeps the original size shape of composite.The ceramics of structural integrity
Layer has preferable fire protecting performance, and it can effectively hinder the transmission of combustible and heat, and then suppress composite inner
The volatilization and loss of material.Therefore, can ceramic coating material before combustion after mechanical property and dimensional stability, for anti-
The performance of fiery effect serves vital effect.
The content of the invention
It is an object of the invention to provide it is a kind of can ceramic epoxy resin fireproof coating, prepare the original of the fireproof coating
Material includes nano-silicon dioxide modified epoxy resin.Nano-silicon dioxide modified epoxy resin is added in coating, can burnt
The structure of ceramic is formed during erosion, the person's movements and expression produced in ablation process is reduced, plays preferable fireproofing function.Need special
Illustrate, nano-silicon dioxide modified epoxy resin herein, the particle diameter for referring to silica is nanoscale.
The mass fraction of silica is 35~45% in the nano-silicon dioxide modified epoxy resin;It is preferred that 40%.
The nano-silicon dioxide modified epoxy resin is prepared by sol-gel process;It is preferred that being purchased from Germany wins wound
The F400 of industrial group.
It is preferred that, preparing the raw material of fireproof coating of the present invention includes epoxy-resin systems, the epoxy resin
System includes base-material and filler, by weight, and base-material includes 0~65 part of non-modified epoxy resin, nano silicon and changed
10~65 parts of epoxy resin of property;Filler includes 5~15 parts of wollastonite, 3~7 parts of mica, 0~4 part of aluminium hydroxide, glass dust 9
~17 parts, 5~11 parts of APP and with 4~12 parts of antimony oxide.
It is preferred that, by weight, base-material includes 0~32 part of non-modified epoxy resin, nano-silicon dioxide modified epoxy
10~42 parts of resin;Filler includes 6~10 parts of wollastonite, 3~5 parts of mica, 1~1.5 part of aluminium hydroxide, glass dust 9~12
Part, 5~7 parts of APP and with 5~7 parts of antimony oxide.
Further preferred, by weight, base-material includes nano-silicon dioxide modified 42 parts of epoxy resin;Wrapped in filler
Include 8 parts of wollastonite, 4 parts of mica, 1.25 parts of aluminium hydroxide, 10 parts of glass dust, 6 parts of APP and with 6 parts of antimony oxide.
Base-material in epoxy-resin systems of the present invention is the main material during fire prevention, and addition wherein is filled out
Material, can further improve the stability in ablation process of base-material, improve final flameproof effect.
It is preferred that, the particle diameter of each component is micron order in the filler, preferably 5~20 μm.Micron-sized filler can be with
Base-material is more preferably mixed, and the fire protecting performance of resulting materials is more preferable.
It is preferred that, the preparation method of the epoxy-resin systems comprises the following steps:
1) stirring at low speed:Sequentially add to be the filler of various filler gross masses 20%~70%, stirring in base-material
Mix and carry out controlling the rotating speed be in device in stirring at low speed, whipping process:1~1.5h, 500~1000r/min;2~2.5h, 2000r/
min;It is 60~80 DEG C to control temperature;
2) high-speed stirred:In the mixture that remaining various fillers are all added to stirring at low speed completion, vacuum is carried out
The rotating speed is controlled to be in high-speed stirred, whipping process:1~1.5h, 500~1000r/min;2~2.5h, 2000~2500r/min;
2~3h, 3500~4000r/min;It is 60~80 DEG C to control temperature;
3) grind:After the completion of high-speed stirred, sample is stood into 24~48h at room temperature, three roller grindings, grinding are then carried out
During:
Spacing pattern, spacing 1:90~75 μm, spacing 2:45~30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60~45 μm, spacing 2:20~15 μm, rotating speed 60r/min, cycle-index 2
It is secondary;Second step:Spacing 1:30~25 μm, spacing 2:10~5 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:
15~10 μm, spacing 2:1~5 μm, rotating speed 60r/min, cycle-index 2 times obtains epoxy-resin systems.
Evenly, performance is more preferable for the mixing of each material of epoxy-resin systems prepared using the above method.
It is preferred that, preparing also includes curing agent methyl tetrahydro phthalic anhydride and dimethylbenzyl in fireproof coating raw material of the present invention
Amine.
It is preferred that, prepare in the fireproof coating raw material, by weight, including:100 parts of epoxy-resin systems, 30~
50 parts of methyl tetrahydro phthalic anhydride and 0.3~0.5 part of dimethyl benzylamine.
Epoxy-resin systems of the present invention are in liquid condition, it is impossible to directly solidify gluing, are added after above-mentioned curing agent
It can be achieved preferably to bond with fireproof material surface need to be carried out.
It is preferred that, the preparation method of this fireproof coating comprises the following steps:By epoxy-resin systems, methyl tetrahydro phthalic anhydride
20~30min is stirred under conditions of speed is 200~500r/min with dimethyl benzylamine, vacuum suction is then carried out to wherein
Bubble all disappear;During the stirring and pumping, it is 60~75 DEG C to control temperature.
It is preferred that, during application, the program curing of the fireproof coating is:90 DEG C, keep 30min;120 DEG C,
Keep 60min;140 DEG C, keep 30min;160 DEG C, keep 120min.
It is preferred that, during application, the coating thickness of the fireproof coating is 500~800 μm.
Fireproof coating of the present invention has the advantages that:
Prepared epoxy resin-matrix fireproof coating thing of the present invention is free of volatile organic content, the chi before and after burning
Preferably, compared to common fireproof silicon/rubber coating system, mechanical property is also higher for very little stability, and this is economical real for research
Have great importance with high performance fireproof coating.
After ablation processes, modified epoxy coating material is changed into ceramic material, and the ceramic material maintains compound
Size and dimension before material ablation.Compared to pure epoxy resin coating material, modified coating material resistance involved in the present invention
Fire performance more preferably, the ceramic material with some strength can be formed after burning, and be intactly covered in substrate surface, serve good
Good heat-insulated and flameproof effect, and then effectively prevent flame persistently to be spread to inside base material.
Brief description of the drawings
Fig. 1 is the form of coating material after ablation;
The surface combustion situation of Fig. 2 planks two.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
The present embodiment is related to epoxy-resin systems of the present invention, is prepared from by the following raw material:
Base-material:Non-modified epoxy resin 31.5g, nano-silicon dioxide modified epoxy resin 10.5g;
Filler:Wollastonite 8g, mica 4g, aluminium hydroxide 1.25g, glass dust 10g, APP 6g, antimony oxide 6g,
The mass fraction of silica is 40% in the nano-silicon dioxide modified epoxy resin.
The preparation flow of the epoxy-resin systems is as follows:
1) by all fillers in vacuum drying oven drying process 2h, drying temperature be 100 DEG C;
2) sequentially add and account in the matrix being made up of non-modified epoxy resin and nano-silicon dioxide modified epoxy resin
The filler of each filler gross mass 50%, carries out stirring at low speed in agitator, and stirring flow is followed successively by:1) 500r/min, 1h;2)
2000r/min, 2h;Whipping process controls temperature to be 60 DEG C.
3) all remaining fillers are added, high-speed vacuum stirring is carried out in agitator, stirring flow is followed successively by:1)
1000r/min, 1h;2) 2000r/min, 2h;3) 3500r/min, 2h.Whipping process controls temperature to be 60 DEG C.
4) stir after the completion of, sample is stood into 36h at room temperature, then carry out three roller grindings so that particle reach it is optimal
Dispersity, three roller grinding technics are as follows:
Spacing pattern, spacing 1:90 μm, spacing 2:30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60 μm, spacing 2:15 μm, rotating speed 60r/min, cycle-index 2 times;Second step:
Spacing 1:30 μm, spacing 2:10 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:15 μm, spacing 2:5 μm, turn
Fast 60r/min, cycle-index 2 times.Obtain epoxy-resin systems.
The present embodiment further relates to include the fireproof coating of above-mentioned epoxy-resin systems, including above-mentioned epoxy-resin systems
0.43~0.47g of 100g, 43~47g of methyl tetrahydro phthalic anhydride and dimethyl benzylamine.
The preparation method of this fireproof coating is:By above-mentioned raw materials rotating speed be 300r/min under conditions of stirring at low speed
20min;Stirring is completed after being evacuated 20min in vacuum drying oven, until sample interior bubble is wholly absent.Stir and vacuumize temperature
Degree is 60 DEG C.
Embodiment 2
The present embodiment is related to epoxy-resin systems of the present invention, is prepared from by the following raw material:
Base-material:Non-modified epoxy resin 21g, nano-silicon dioxide modified epoxy resin 21g;
Filler:Wollastonite 8g, mica 4g, aluminium hydroxide 1.25g, glass dust 10g, APP 6g, antimony oxide 6g;
The mass fraction of silica is 40% in the nano-silicon dioxide modified epoxy resin.
The preparation flow of the epoxy-resin systems is as follows:
1) by all fillers in vacuum drying oven drying process 2h, drying temperature be 100 DEG C;
2) sequentially add and account in the base-material being made up of non-modified epoxy resin and nano-silicon dioxide modified epoxy resin
The filler of each filler gross mass 50%, carries out stirring at low speed in agitator, and stirring flow is followed successively by:1) 500r/min, 1h;2)
2000r/min, 2h;Whipping temp is 70 DEG C.
3) all remaining fillers are added, high-speed vacuum stirring is carried out in agitator, stirring flow is followed successively by:1)
1000r/min, 1h;2) 2000r/min, 2.5h;3) 4000r/min, 2h.Whipping temp is 70 DEG C.
4) stir after the completion of, sample is stood into 36h at room temperature, then carry out three roller grindings so that particle reach it is optimal
Dispersity, three roller grinding technics are as follows:
Spacing pattern, spacing 1:90 μm, spacing 2:30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60 μm, spacing 2:15 μm, rotating speed 60r/min, cycle-index 2 times;Second step:
Spacing 1:30 μm, spacing 2:10 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:15 μm, spacing 2:5 μm, turn
Fast 60r/min, cycle-index 2 times.Obtain epoxy-resin systems.
The present embodiment further relates to include the fireproof coating of above-mentioned epoxy-resin systems, including above-mentioned epoxy-resin systems
100g, 39~44g of methyl tetrahydro phthalic anhydride and dimethyl benzylamine 0.39-0.44g.
The preparation method of this fireproof coating is:By above-mentioned raw materials under conditions of 500r/min stirring at low speed 25min;Stir
Completion is mixed after being evacuated 30min in vacuum drying oven, until sample interior bubble is wholly absent.Stirring and vaporization temperature are 70
℃。
Embodiment 3
The present embodiment is related to epoxy-resin systems of the present invention, is prepared from by the following raw material:
Base-material:Non-modified epoxy resin 31.5g, nano-silicon dioxide modified epoxy resin 10.5g;
Filler:Wollastonite 8g, mica 4g, aluminium hydroxide 1.25g, glass dust 10g, APP 6g, antimony oxide 6g,
The mass fraction of silica is 40% in the nano-silicon dioxide modified epoxy resin.
The preparation technology flow of above-mentioned epoxy-resin systems is as follows:
1) all fillers are placed in drying process 2h in vacuum drying oven, 100 DEG C of temperature;
2) sequentially added in the matrix being made up of non-modified epoxy resin and nano-silicon dioxide modified epoxy resin for
The filler of each filler gross mass 50%, carries out stirring at low speed in agitator, and stirring flow is followed successively by:1) 500r/min, 1.5h;
2) 2000r/min, 2.5h;Whipping temp is 75 DEG C.
3) remaining whole fillers are added, high-speed vacuum stirring is carried out in agitator, stirring flow is followed successively by:1)
1000r/min, 1.5h;2) 2000r/min, 2.5h;3) 4000r/min, 2.5h.Whipping temp is 75 DEG C.
4) stir after the completion of, sample is stood into 48h at room temperature, then carry out three roller grindings so that particle reach it is optimal
Dispersity, three roller grinding technics are as follows:
Spacing pattern, spacing 1:90 μm, spacing 2:30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60 μm, spacing 2:15 μm, rotating speed 60r/min, cycle-index 2 times;Second step:
Spacing 1:30 μm, spacing 2:10 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:15 μm, spacing 2:5 μm, turn
Fast 60r/min, cycle-index 2 times.Obtain epoxy-resin systems.
The present embodiment further relates to include the fire proofing material of this epoxy-resin systems, including above-mentioned epoxy-resin systems
0.34~0.38g of 100g, 34~38g of methyl tetrahydro phthalic anhydride and dimethyl benzylamine.
The preparation method of this fireproof coating is:Above-mentioned raw materials are stirred into 30min under conditions of 500r/min;Stir
Into after being evacuated 40min in vacuum drying oven, until sample interior bubble is wholly absent.The temperature for stirring and vacuumizing is 70
℃。
Embodiment 4
The present embodiment is related to epoxy-resin systems of the present invention, is prepared from by the following raw material:
Base-material:Nano-silicon dioxide modified 42 parts of epoxy resin;
Filler:8 parts of wollastonite, 4 parts of mica, 1.25 parts of aluminium hydroxide, 10 parts of glass dust, 6 parts of APP, three oxidations two
6 parts of antimony.
The preparing technique process flow of above-mentioned epoxy-resin systems is as follows:
1) all fillers are placed in drying process 2h in vacuum drying oven, 100 DEG C of temperature;
2) sequentially added in nano-silicon dioxide modified epoxy resin base-material as the filler of each filler gross weight 50%, in
Stirring at low speed is carried out in agitator, stirring flow is followed successively by:1) 500r/min, 1.5h;2) 2000r/min, 2.5h;Whipping temp
For 80 DEG C.
3) filler of residual mass is added, high-speed vacuum stirring is carried out in agitator, stirring flow is followed successively by:1)
1000r/min, 1.5h;2) 2000r/min, 2.5h;3) 4000r/min, 3h.Whipping temp is 80 DEG C.
4) stir after the completion of, sample is stood into 48h at room temperature, then carry out three roller grindings so that particle reach it is optimal
Dispersity, three roller grinding technics are as follows:
Spacing pattern, spacing 1:90 μm, spacing 2:30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60 μm, spacing 2:15 μm, rotating speed 60r/min, cycle-index 2 times;Second step:
Spacing 1:30 μm, spacing 2:10 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:15 μm, spacing 2:5 μm, turn
Fast 60r/min, cycle-index 2 times.Obtain epoxy-resin systems.
The present embodiment further relates to include the fireproof coating of this epoxy-resin systems, including:
Above-mentioned epoxy-resin systems 100g, 0.3~0.34g of 30~34g of methyl tetrahydro phthalic anhydride and dimethyl benzylamine;
The preparation method of this fireproof coating is:The stirring at low speed 40min under conditions of 400r/min;Stirring complete after
50min is evacuated in vacuum drying oven, until sample interior bubble is wholly absent.Stirring and vaporization temperature are 75 DEG C.
Embodiment 5
The present embodiment is related to the curing of coating material described in Claims 1 to 4, comprises the following steps:
By the coating material described in embodiment 1~4 in 90 DEG C, 30min;120 DEG C, 60min;140 DEG C, 30min;160 DEG C,
Heat stepwise is carried out under conditions of 120min.
Comparative example 1
Compared with embodiments herein, without nano-silicon dioxide modified epoxy resin and filler in this comparative example;
Include the raw material of following parts by weight:100 parts of non-modified epoxy resin, methyl tetrahydro phthalic anhydride (92 parts) and dimethyl
Benzylamine (0.92 part).
Preparing technique process flow is as follows:
Weigh epoxy resin, methyl tetrahydro phthalic anhydride and dimethyl benzylamine, stirring at low speed 20min;Stirring is completed after true
30min is evacuated in empty baking oven, until sample interior bubble is wholly absent.Stirring and vaporization temperature are 60 DEG C.
Comparative example 2
This comparative example also relates to a kind of fire resistant coating material, compared with embodiment 1~4, and its difference is, epoxy resin
System is prepared in base-material without nano-silicon dioxide modified epoxy resin, and the base-material is 42g non-modified epoxy resin.
Experimental example 1
The ablation property of coating material described in embodiment 1~4 and comparative example 1~2 and thermal stability test.
Ablation is carried out to the material of embodiment 1~4 and the gained of comparative example 1~2, the compression performance before and after ablation is according to standard
ASTM D695 are tested, 25 DEG C of temperature, compression speed 0.001s-1.Ablating technics flow is as follows:
(1) take out the sample after solidification in a mold (can design corresponding mould according to the geomery of solidified sample
Specification).
(2) it is put into Muffle furnace;Air atmosphere ablation, heating rate is 10 DEG C/min.
(3) reach after required ablation temperature (650-950 DEG C), be incubated 0.5-2.5h, then natural cooling is down to room temperature.
Volume ratio before and after ablation, is calculated according to formula 1.
Wherein, V1And V2Respectively represent ablation before and after cylindrical sample apparent volume.
Form is shown in Fig. 1, Fig. 1 after the coating material ablation of embodiment 1~4 and comparative example 2, from left to right, is followed successively by pair
It is changed into ashes after the form after coating material ablation in ratio 2 and embodiment 1~4, the material ablation of comparative example 1, does not possess
Solid shape.
Thermal stability test is carried out to the coating material of embodiment 1~4 and comparative example 2, it is (beautiful using thermogravimetric analyzer
State, TA Q500 types) tested, example weight 5-10mg, 10 DEG C/min of heating rate, air atmosphere.
Combustibility is tested according to standard ASTM D7309-11.Contrast the combustibility test knot in Tables 1 and 2
Fruit understand, the fire resistance of embodiment coating material apparently higher than comparative example, wherein, maximum HRR value can be reduced to
0.25 times of comparative example 1, specific Heat liberation unit can be reduced to 0.4 times of comparative example 1, and residue decomposition ratio can improve to
More than 20 times of comparative example 1.
The embodiment the performance test results of table 1.
1Represent 650 DEG C, ablation processes 1.5h;
2Represent 950 DEG C, ablation processes 1.5h;
Indicate:When volume after combustion change is more than 20%, it is impossible to accurately measure its compressive strength.
The combustibility test result of 2. comparative example of table 1
Because the material in comparative example 1 is burnt down completely, basic noresidue, i.e. residue decomposition ratio are zero, it is impossible to determine it
Mechanical property, can only determine above-mentioned several indexs.
Experimental example 2
The present embodiment is related to effect of the fire resistant coating material in embodiment 4 and comparative example 1 in actually fire prevention and compared.
Concrete operations are:The common plank for remove dirt, polishing smooth, the fireproof coating in embodiment 4 and comparative example 1 is equal
On the surface for being coated on plank side evenly, curing molding then is carried out according to the method in embodiment 5, obtains being coated on pawpaw
The smooth white coating on surface.
The fire prevention of coating material, heat-proof quality are tested as follows.Will be made in embodiment 4 and comparative example 1
Standby plank is placed on iron stand, wherein, there is flame envelope of the side surface of coating one just to alcohol blast burner.Light after alcolhol burner, use
Infrared temperature analyzer is tested plank and changed with time situation away from flame side centre of surface point temperature.The burning feelings of plank
In condition such as Fig. 2, Fig. 2, superposed two width figure is that the coating in comparative example 1 is applied to the result after the after-combustion of surface, wherein left
Side figure is the situation for the plank burning for scribbling coating, and right part of flg is the back side after burning, and the two width figures positioned at bottom are embodiment 4
In coating be applied to the result after surface combustion, wherein left hand view is the plank combustion case for scribbling coating, and right part of flg is burning
The back side afterwards, as seen from the figure, the ceramic layer formed after the coating material burning in embodiment 4 are intactly covered in plank table
Face, the positive blackening of plank burning is in confused situation aobvious, and the back side of burning does not have a blackening substantially, and the coating plank in comparative example 1
The blackening situation of front and back is very serious, it can thus be seen that the coating of the application can effectively prevent flame to wood
Intralamellar part quickly spreads, the speed for preventing plank opposite side surface temperature to rise, and serves fire-retardant, heat-insulated well and fire prevention
Effect.
Although above having made to retouch in detail to the present invention with general explanation, embodiment and experiment
State, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, are belonged to claimed
Scope.
Claims (10)
1. it is a kind of can ceramic epoxy resin fireproof coating, it is characterised in that preparing the raw material of the fireproof coating includes
Nano-silicon dioxide modified epoxy resin.
2. fireproof coating according to claim 1, it is characterised in that two in the nano-silicon dioxide modified epoxy resin
The mass fraction of silica is 35~45%.
3. fireproof coating according to claim 1 or 2, it is characterised in that preparing the raw material of the fireproof coating includes
Epoxy-resin systems, the epoxy-resin systems include base-material and filler, by weight, and base-material includes non-modified asphalt mixtures modified by epoxy resin
0~65 part of fat, 10~65 parts of nano-silicon dioxide modified epoxy resin;Filler includes 5~15 parts of wollastonite, mica 3~7
Part, 0~4 part of aluminium hydroxide, 9~17 parts of glass dust, 5~11 parts of APP and with 4~12 parts of antimony oxide.
4. fireproof coating according to claim 3, it is characterised in that by weight, base-material includes non-modified asphalt mixtures modified by epoxy resin
0~32 part of fat, 10~42 parts of nano-silicon dioxide modified epoxy resin;Filler includes 6~10 parts of wollastonite, mica 3~5
Part, 1~1.5 part of aluminium hydroxide, 9~12 parts of glass dust, 5~7 parts of APP and with 5~7 parts of antimony oxide.
5. the fireproof coating according to claim 3 or 4, it is characterised in that the particle diameter of each component is micro- in the filler
Meter level, preferably 5~20 μm.
6. the fireproof coating according to any one of claim 3~5, it is characterised in that the preparation of the epoxy-resin systems
Method comprises the following steps:
1) stirring at low speed:Sequentially added in base-material be various filler gross masses 20%~70% partial filler, stirring
Carry out controlling the rotating speed be in device in stirring at low speed, whipping process:1~1.5h, 500~1000r/min;2~2.5h, 2000r/
min;It is 60~80 DEG C to control temperature;
2) high-speed stirred:In the mixture that remaining various fillers are all added to stirring at low speed completion, vacuum is carried out at a high speed
Stirring, controls in whipping process the rotating speed to be:1~1.5h, 500~1000r/min;2~2.5h, 2000~2500r/min;2~
3h, 3500~4000r/min;It is 60~80 DEG C to control temperature;
3) grind:After the completion of high-speed stirred, sample is stood into 24~48h at room temperature, three roller grindings, process of lapping are then carried out
In:
Spacing pattern, spacing 1:90~75 μm, spacing 2:45~30 μm, rotating speed 100r/min, cycle-index 2 times;
Pressure pattern, the first step:Spacing 1:60~45 μm, spacing 2:20~15 μm, rotating speed 60r/min, cycle-index 2 times;The
Two steps:Spacing 1:30~25 μm, spacing 2:10~5 μm, rotating speed 60r/min, cycle-index 2 times;3rd step, spacing 1:15~10
μm, spacing 2:1~5 μm, rotating speed 60r/min, cycle-index 2 times obtains epoxy-resin systems.
7. the fireproof coating according to any one of claim 1~6, it is characterised in that prepare the raw material of the fireproof coating
In also include curing agent methyl tetrahydro phthalic anhydride and dimethyl benzylamine.
8. fireproof coating according to claim 7, it is characterised in that prepare in the fireproof coating raw material, by weight,
Including:100 parts of epoxy-resin systems, 30~50 parts of methyl tetrahydro phthalic anhydride and 0.3~0.5 part of dimethyl benzylamine.
9. the preparation method of fireproof coating described in claim 7 or 8, it is characterised in that comprise the following steps:By epoxy resin body
System, methyl tetrahydro phthalic anhydride and dimethyl benzylamine stir 20~30min, Ran Houjin under conditions of speed is 200~500r/min
Row vacuum suction all disappears to bubble therein;During the stirring and pumping, it is 60~75 DEG C to control temperature.
10. application of the fireproof coating described in claim 7 or 8 in fire prevention, it is preferred that needing the painting of fireproof material surface
Thickness is covered for 500~800 μm.
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CN109868032A (en) * | 2019-01-22 | 2019-06-11 | 江苏冠军科技集团股份有限公司 | A kind of fireproof flame-retardant coating and preparation method thereof based on microencapsulation technology |
CN110054968A (en) * | 2019-05-21 | 2019-07-26 | 张志广 | A kind of microcapsules ceramic fireproof coating and its preparation process |
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