CN114316736A - Solvent-free epoxy intumescent fire-retardant coating and preparation method thereof - Google Patents
Solvent-free epoxy intumescent fire-retardant coating and preparation method thereof Download PDFInfo
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- CN114316736A CN114316736A CN202111593099.7A CN202111593099A CN114316736A CN 114316736 A CN114316736 A CN 114316736A CN 202111593099 A CN202111593099 A CN 202111593099A CN 114316736 A CN114316736 A CN 114316736A
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- chlorinated paraffin
- pentaerythritol
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- 238000000576 coating method Methods 0.000 title claims abstract description 54
- 239000004593 Epoxy Substances 0.000 title claims abstract description 53
- 239000011248 coating agent Substances 0.000 title claims abstract description 50
- 239000003063 flame retardant Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000012188 paraffin wax Substances 0.000 claims abstract description 60
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 12
- 239000003822 epoxy resin Substances 0.000 claims abstract description 12
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 12
- 239000003085 diluting agent Substances 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 11
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 9
- 229940059574 pentaerithrityl Drugs 0.000 claims description 53
- 239000000203 mixture Substances 0.000 claims description 35
- 239000006185 dispersion Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000012046 mixed solvent Substances 0.000 claims description 11
- -1 alkyl glycidyl ether Chemical compound 0.000 claims description 10
- 239000004952 Polyamide Substances 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229920002647 polyamide Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 6
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical group CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- 229920006231 aramid fiber Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- SHKUUQIDMUMQQK-UHFFFAOYSA-N 2-[4-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COCCCCOCC1CO1 SHKUUQIDMUMQQK-UHFFFAOYSA-N 0.000 claims description 3
- WTYYGFLRBWMFRY-UHFFFAOYSA-N 2-[6-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COCCCCCCOCC1CO1 WTYYGFLRBWMFRY-UHFFFAOYSA-N 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 abstract description 9
- 239000010959 steel Substances 0.000 abstract description 9
- 230000007062 hydrolysis Effects 0.000 abstract description 4
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- 238000005260 corrosion Methods 0.000 abstract description 2
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- 229910052799 carbon Inorganic materials 0.000 description 8
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
- 239000004088 foaming agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000007790 scraping Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000009041 PM 40 Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 1
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229920003319 Araldite® Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
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- DMKSVUSAATWOCU-HROMYWEYSA-N loteprednol etabonate Chemical compound C1CC2=CC(=O)C=C[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)OCCl)(OC(=O)OCC)[C@@]1(C)C[C@@H]2O DMKSVUSAATWOCU-HROMYWEYSA-N 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention relates to a solvent-free epoxy intumescent fire-retardant coating and a preparation method thereof, belonging to the field of coatings. The solvent-free epoxy intumescent fire retardant coating A component consists of 10-30 parts by mass of epoxy resin, 5-15 parts by mass of diluent, 0.3-0.8 part by mass of defoaming agent, 0.1-3 parts by mass of adhesion promoter, 5-20 parts by mass of chlorinated paraffin coated pentaerythritol, 20-40 parts by mass of acid donor, 6-15 parts by mass of inorganic nano filler, 1-6 parts by mass of reinforcing fiber and 0.1-1 part by mass of rheological agent; the component B is an epoxy curing agent, and the component A and the component B are uniformly mixed for use. The chlorinated paraffin-coated pentaerythritol prepared by the invention improves the hydrolysis resistance and the thermal stability of pentaerythritol, has excellent humidity resistance and heat resistance when being applied to solvent-free epoxy intumescent fire-retardant coating, can be widely applied to fire protection of indoor and outdoor steel structures, is green and environment-friendly, and has excellent fire resistance reliability, corrosion resistance and excellent mechanical properties.
Description
Technical Field
The invention relates to a solvent-free epoxy intumescent fire-retardant coating and a preparation method thereof, belonging to the field of functional coatings.
Background
The intumescent fire-retardant coating for the steel structure is a functional coating suitable for fire-resistant protection of large-scale steel structures indoors and outdoors, can expand to generate a low-heat-conduction carbon layer after being fired, and can avoid the collapse of a building caused by the loss of mechanical strength due to the too fast temperature rise of steel in a fire scene, thereby providing safe evacuation crowd and fire-fighting retention time for the building after the fire disaster occurs.
The typical effective components of the intumescent steel structure fireproof coating comprise a film forming material, a carbon forming agent, an acid donor and a gas donor, wherein the carbon forming agent is mainly hydrocarbon, can react with acid at high temperature to dehydrate and form carbon, and is a main part of an intumescent thermal insulation layer.
The most commonly used carbon forming agent at present is mainly pentaerythritol, but the carbon forming agent has the problem of easy hydrolysis, and the carbon forming agent gradually loses the problem of influencing the practical applicability of the fireproof coating in the using process of the fireproof coating. The chlorinated paraffin is an organic substance, is a chlorinated derivative of paraffin, and has the advantages of low volatility, good water resistance, flame retardance, good electrical insulation, low price, low toxicity and the like. The flame-retardant intumescent flame-retardant foaming agent is often applied to intumescent fire-retardant coatings, and on one hand, the flame-retardant intumescent flame-retardant foaming agent can play a role in gas-phase flame retardance and can also be used as an auxiliary foaming agent (gas donor) to participate in the foaming process of the intumescent fire-retardant coatings. Meanwhile, the chlorinated paraffin also has a certain physical barrier effect, and a formed solid film is not hydrophilic and can isolate and reduce heat source radiation.
Disclosure of Invention
The invention aims to provide a solvent-free epoxy intumescent fire retardant coating and a preparation method thereof, wherein chlorinated paraffin coated pentaerythritol is applied to the solvent-free epoxy intumescent fire retardant coating, the method has simple process and easily obtained materials, and the prepared coating has excellent fire resistance and reliable performance.
The technical scheme of the invention is as follows:
a solvent-free epoxy intumescent fire retardant coating comprises the following components in parts by weight:
the component A comprises:
and B component:
140-60 parts of an epoxy curing agent;
210-40 parts of an epoxy curing agent;
310-40 parts of an epoxy curing agent.
The solvent-free epoxy intumescent fire retardant coating comprises a component A: the epoxy resin is one or a mixture of more than two of E51 and standard liquid bisphenol F epoxy resin;
the diluent is one or a mixture of more than two of C12-14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether and 1, 6-hexanediol diglycidyl ether;
the defoaming agent is foam-breaking polysiloxane or polymer defoaming agent without organosilicon;
the adhesion promoter is one or more of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-aminopropyl triethoxy silane and gamma-methacryloxypropyl trimethoxy silane;
the acid donor is II type ammonium polyphosphate with polymerization degree more than 1000;
the inorganic nano-filler is one or a mixture of more than two of nano rutile type titanium dioxide, nano zinc oxide, nano aluminum hydroxide and nano magnesium hydroxide;
the reinforced fiber is one or a mixture of more than two of carbon fiber, carbon nano tube, aramid fiber, glass fiber and silicate fiber;
the rheological agent is one or two of liquid polyamide wax, bentonite rheological agent and fumed silica.
In the solvent-free epoxy intumescent fire-retardant coating, in the component A, the preparation method of chlorinated paraffin-coated pentaerythritol comprises the following steps:
(1) putting chlorinated paraffin into an environment-friendly mixed solvent under the stirring condition of the rotating speed of 200-500 rpm, and stirring until the chlorinated paraffin is completely dissolved to form a chlorinated paraffin solution with the mass fraction of 10-30%;
(2) according to the mass ratio of 1 (1-5) of chlorinated paraffin to pentaerythritol, putting pentaerythritol powder into a chlorinated paraffin solution under the stirring condition of the rotating speed of 400-500 rpm, and increasing the rotating speed to 1500-2000 rpm until the mixture is uniformly stirred;
(3) rotationally evaporating the obtained mixture at 50-60 ℃, removing the mixed solvent, placing the mixture in an oven, and fully drying to obtain a chlorinated paraffin-coated pentaerythritol mixture;
(4) and grinding the chlorinated paraffin-coated pentaerythritol mixture by a ball mill until the average particle size reaches 40 mu m to obtain the micropowder-grade chlorinated paraffin-coated pentaerythritol.
The solvent-free epoxy intumescent fire-retardant coating adopts the propylene glycol butyl ether and the dearomatized hydrocarbon solvent oil with the mass ratio of 1:1 as the environment-friendly mixed solvent.
The solvent-free epoxy intumescent fire retardant coating adopts one or a mixture of more than two of chlorinated paraffin with chlorine content of 38-42 wt%, 48-52 wt% and 68-72 wt%.
The solvent-free epoxy intumescent fire-retardant coating is prepared by mixing pentaerythritol with the maximum particle size of 40 mu m.
In the solvent-free epoxy intumescent fire-retardant coating, in the component B, the epoxy curing agent is one or a mixture of more than two of modified polyamide, modified alicyclic amine and polyether amine, and the epoxy curing agent 1, the epoxy curing agent 2 and the epoxy curing agent 3 are respectively selected from different epoxy curing agents.
The solvent-free epoxy intumescent fire retardant coating is prepared by the following steps in the following sequence:
the component A comprises:
(1) placing epoxy resin and a diluent in a dispersion tank, adding a defoaming agent and an adhesion promoter at the rotating speed of 500-800 rpm, and dispersing for 5-10 minutes;
(2) placing chlorinated paraffin-coated pentaerythritol, an acid donor, inorganic nano-filler, reinforcing fiber and a rheological agent in a dispersion tank in sequence, adjusting the dispersion speed to 1800-2000 rpm, starting a water bath cooling device, ensuring that the temperature of the material is lower than 60 ℃, and dispersing for 30-40 minutes;
and B component: the curing agent is mixed and dispersed for 5 to 10 minutes at a rotating speed of 200 to 300 rpm.
The design idea of the invention is as follows:
according to the invention, a microcapsule coating technical method is adopted, chlorinated paraffin with excellent water resistance is used as a capsule material for coating easily-hydrolyzed pentaerythritol, the prepared chlorinated paraffin-coated pentaerythritol is introduced into the solvent-free epoxy intumescent fire-retardant coating, the prepared paint film has excellent humidity resistance and heat resistance, and the introduction of the chlorinated paraffin also improves the overall fire resistance of the coating.
Compared with the prior commercially available product technology, the invention has the advantages and beneficial effects that:
1. the chlorinated paraffin-coated pentaerythritol provided by the method is coated by the chlorinated paraffin, so that the compatibility of the chlorinated paraffin-coated pentaerythritol with a polymer is improved, the loss conditions of hydrolysis and pyrolysis of the pentaerythritol in the use process of the fireproof coating are improved, and the durability of the fireproof coating is improved.
2. The chlorinated paraffin coated pentaerythritol provided by the method can be used as a synergistic foaming agent to generate a good synergistic flame retardant effect with carbon forming agent pentaerythritol and acid source ammonium polyphosphate, and the fire resistance protection performance of the fireproof coating on a steel structure is improved.
3. The chlorinated paraffin-coated pentaerythritol provided by the method has the advantages of wide material source, low price, easy obtainment and simple preparation method, and is suitable for industrial production.
4. The chlorinated paraffin-coated pentaerythritol prepared by the invention improves the hydrolysis resistance and the thermal stability of pentaerythritol, has excellent humidity resistance and heat resistance when being applied to solvent-free epoxy intumescent fire-retardant coating, can be widely applied to fire protection of indoor and outdoor steel structures, is green and environment-friendly, and has excellent fire resistance reliability, corrosion resistance and excellent mechanical properties.
Detailed Description
In the specific implementation process, the preparation method of the chlorinated paraffin-coated pentaerythritol comprises the following steps: firstly, adding selected chlorinated paraffin into a mixed solvent according to a specified amount under the condition of high-speed stirring, stirring until the chlorinated paraffin is completely dissolved, then adding pentaerythritol under the condition of stirring and fully stirring, then heating to evaporate and remove solvent components, fully drying, and then grinding evaporation residues to a specified fineness to obtain the chlorinated paraffin coated pentaerythritol. Preparing a solvent-free epoxy intumescent fire retardant coating: the solvent-free epoxy intumescent fire retardant coating A component consists of 10-30 parts by mass of epoxy resin, 5-15 parts by mass of diluent, 0.3-0.8 part by mass of defoaming agent, 0.1-3 parts by mass of adhesion promoter, 5-20 parts by mass of chlorinated paraffin coated pentaerythritol, 20-40 parts by mass of acid donor, 6-15 parts by mass of inorganic nano filler, 1-6 parts by mass of reinforcing fiber and 0.1-1 part by mass of rheological agent; the component B is an epoxy curing agent, and the component A and the component B are uniformly mixed for use.
Wherein:
the epoxy resin is one or a mixture of more than two of E51 and standard liquid bisphenol F epoxy resin.
The diluent is one or a mixture of more than two of C12-14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether and 1, 6-hexanediol diglycidyl ether.
The defoaming agent is a defoaming polysiloxane or polymer defoaming agent without organic silicon. Preferably, the foam breaking type polysiloxane or polymer non-silicone defoaming agent can be one or more of BYK-066N, BYK-A506, BYK-054, BYK-057 of Bikko company or Tego Airex 900 of Digao company, and the defoaming agents are all suitable for defoaming of the system and have excellent stability.
The adhesion promoter is one or more of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-aminopropyl triethoxy silane and gamma-methacryloxypropyl trimethoxy silane. Preferably, the adhesion promoter can be one or more than two of Silquest A-187, Silquest A-174 and Silquest A-1100 of the American Meighur company, and can enhance the adhesion of the solvent-free nano epoxy intumescent fire retardant coating to the substrate.
The chlorinated paraffin used for the chlorinated paraffin-coated pentaerythritol can be one or a mixture of more than two of chlorinated paraffins with chlorine content of 38-42%, 48-52% and 68-72%. Preferably, the grade of the chlorinated paraffin is CP-70 with the chlorine content of 70-72%. The environment-friendly mixed solvent adopts propylene glycol butyl ether and dearomatized hydrocarbon solvent oil with the mass ratio of 1: 1. Preferably, the dearomatized hydrocarbon solvent oil can be Exxsol D30 from Exxon Mobil. The pentaerythritol type may be 98% purity monopentaerythritol, dipentaerythritol, or a mixture of the two. Preferably, monopentaerythritol is used which has a particle size of pentaerythritol of at most 40 μm. Preferably, the mono-pentaerythritol grade used may be boston PM-40, DP-40 or Hubei optimized purity 98 wt% micropowder grade mono-pentaerythritol.
The acid donor type is ammonium polyphosphate II with polymerization degree of more than 1000. Preferably, the ammonium polyphosphate used has an average particle size of 40 μm; preferably, the polyphosphoric acid amine can be melamine resin coated modified polyphosphoric acid amine coated by epoxy resin; preferably, FR CROS 486 and FR CROS 584 from Borden, AP-422 and AP-462 from Clariant, and APP-224 and APP-262 from Poseofu are used.
The inorganic nano-filler can be one or a mixture of more than two of nano rutile type titanium dioxide, nano zinc oxide, nano aluminum hydroxide and nano magnesium hydroxide.
The reinforcing fiber can be one of carbon fiber, carbon nano tube, aramid fiber, glass fiber and silicate fiber or a mixture of more than two of the carbon fiber, the carbon nano tube, the aramid fiber, the glass fiber and the silicate fiber.
The rheological agent is one or a mixture of two of liquid polyamide wax, bentonite rheological agent and fumed silica; preferably, one or more of Crayvallac MT rheological agent of Arkema, Bentonie SD-2 rheological agent of Hamming modesty and fumed silica AEROSIL R972 of Wiegenkegsai can be adopted, and the system has good anti-settling property, excellent shear thinning property and anti-sagging property.
The curing agent is one or a mixture of more than two of modified polyamide, modified alicyclic amine and polyether amine.
The technical solutions of the present invention will be further described with reference to the following embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The parts indicated in the examples are, unless otherwise specified, parts by weight.
The relevant raw materials used in the examples and comparative examples were purchased commercially and specified in the following table:
| raw material | Number plate |
| Epoxy resin | NPEL-128 |
| Mixed solvent | Propylene glycol butyl Ether/Exxsol D30 |
| Diluent | Araldite DY 025 |
| Chlorinated paraffin | CP-70 with chlorine content of 70-72 wt% |
| Defoaming agent | BYK-057 |
| Adhesion promoter | Silquest A-1100 |
| Mono-pentaerythritol | Charmor PM-40 |
| Acid donors | FRCROS 486 ammonium polyphosphate |
| Inorganic nano filler | RCL-69 nano-grade rutile type titanium dioxide |
| Reinforcing fiber | LapinusCF730 fiber |
| Rheological agent | AEROSILR972 gas silicon |
| Epoxy curing agent 1 | Ancamide-350A polyamide |
| Epoxy curing agent 2 | IPDA curing agent |
| Epoxy curing agent 3 | T403 curing agent |
Example 1
In this embodiment, the preparation method of chlorinated paraffin-coated pentaerythritol comprises:
(1) under the stirring condition of the rotating speed of 300rpm, a predetermined amount of chlorinated paraffin CP-70 (mass ratio is 20%) is added into a mixture of propylene glycol butyl ether and Exxsol D30 according to the mass ratio of 1:1 (the mass percentage is 80 percent) in the mixed solvent, and stirring until the chlorinated paraffin is completely dissolved to obtain a chlorinated paraffin solution with the mass fraction of 20 percent.
(2) Putting the pentaerythritol powder with the formula amount into a chlorinated paraffin solution with the mass fraction of 20% under the stirring condition of the rotating speed of 500rpm, increasing the rotating speed to 1800rpm, and stirring for 30 minutes until the mixture is uniformly stirred.
(3) The obtained mixture is subjected to rotary evaporation at 60 ℃, the mixed solvent is removed, and the mixture is placed in an oven to be fully dried to obtain evaporation residues, namely: chlorinated paraffin-coated pentaerythritol mixtures.
(4) And grinding the evaporation residue by a ball mill until the average particle size is 40 mu m to obtain the micro-powder chlorinated paraffin-coated pentaerythritol.
In this embodiment, the preparation method of the solvent-free nano epoxy intumescent fire retardant coating is performed according to the following sequence and steps:
the component A comprises:
(1) placing epoxy resin and a diluent in a dispersion tank, adding a defoaming agent and an adhesion promoter at the rotating speed of 600rpm, and dispersing for 10 minutes;
(2) placing chlorinated paraffin-coated pentaerythritol, an acid donor, inorganic nano-filler, reinforcing fiber and a rheological agent in a dispersion tank in sequence, adjusting the dispersion speed to 2000rpm, simultaneously starting an edge scraping device, and timely starting a water bath cooling device to ensure that the temperature of the material is lower than 60 ℃ and dispersing for 30 minutes;
and B component: the curing agent was mixed and dispersed for 10 minutes at 200 rpm.
The components and contents in the examples and comparative examples are specifically illustrated in the following table in parts by mass:
comparative example 1
The difference from example 1 is that chlorinated paraffin CP-70 is added separately in the same amount as the chlorinated paraffin used for coating pentaerythritol in example 1, and monopentaerythritol Charmor PM40 in comparative example 1 is also used in the same amount as in example 1. The preparation process comprises the following steps:
the component A comprises:
(1) placing epoxy resin and a diluent in a dispersion tank, adding a defoaming agent and an adhesion promoter at the rotating speed of 600rpm, and dispersing for 10 minutes;
(2) sequentially placing chlorinated paraffin, pentaerythritol, an acid donor, inorganic nano filler, reinforcing fiber and a rheological agent in a dispersion tank, adjusting the dispersion speed to 2000rpm, simultaneously starting an edge scraping device, and timely starting a water bath cooling device to ensure that the temperature of the material is lower than 60 ℃ and the material is dispersed for 30 minutes;
and B component: the curing agent was mixed and dispersed for 10 minutes at 200 rpm.
Comparative example 2:
the main difference from example 1 is that no chlorinated paraffin CP-70 was added in comparative example 2, and the amount of monopentaerythritol Charmor PM40 was also consistent with the amount used in example 1. The preparation process comprises the following steps:
the component A comprises:
(1) placing epoxy resin and a diluent in a dispersion tank, adding a defoaming agent and an adhesion promoter at the rotating speed of 600rpm, and dispersing for 10 minutes;
(2) putting pentaerythritol, an acid donor, inorganic nano-filler, reinforcing fiber and a rheological agent in a dispersion tank in sequence, adjusting the dispersion speed to 2000rpm, simultaneously starting an edge scraping device, and timely starting a water bath cooling device to ensure that the temperature of the material is lower than 60 ℃ and the material is dispersed for 30 minutes;
and B component: the curing agent was mixed and dispersed for 10 minutes at 200 rpm.
The fire resistance tests of the solvent-free epoxy intumescent steel structure fire-retardant coating prepared in the embodiment 1 and the comparative examples 1-2 are carried out, and the relevant test results are shown in the following table (the fire resistance tests are tested by adopting a rapid test device for the medium-navigation fire-retardant coating, and the dry film thickness of the fire-retardant coating is 1.2 mm);
as can be seen from the relevant experimental data of the example 1 and the comparative examples 1-2, the chlorinated paraffin-coated pentaerythritol prepared by the invention effectively improves the damp-heat resistance of a coating system, and the fire resistance attenuation value of the prepared solvent-free fireproof coating before and after the damp-heat resistance test is less than 13.2%, and the performance is improved by about 16% compared with that of the common pentaerythritol. Compared with the comparative examples 1 and 1-2, the chlorinated paraffin introduced by the capsule wall material also has a synergistic flame retardant effect, the fire resistance is improved from 29min to 38min, and the fire resistance is improved by 31%. The experimental results of the embodiment 1 and the comparative example show that the solvent-free epoxy fire-retardant coating prepared by the invention has excellent wet-heat-aging-resistant performance, can be effectively applied to fire-resistant protection of indoor and outdoor steel structures, has great performance advantages compared with the traditional intumescent fire-retardant coating, and has excellent practical application value.
The above-described embodiments are merely illustrative of the present invention and are not to be construed as limiting the scope of the invention or as limiting the structure of the invention in any way. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (8)
1. The solvent-free epoxy intumescent fire retardant coating is characterized by comprising the following components in parts by weight:
the component A comprises:
and B component:
140-60 parts of an epoxy curing agent;
210-40 parts of an epoxy curing agent;
310-40 parts of an epoxy curing agent.
2. A solventless epoxy intumescent fire retardant coating according to claim 1 wherein in component a: the epoxy resin is one or a mixture of more than two of E51 and standard liquid bisphenol F epoxy resin;
the diluent is one or a mixture of more than two of C12-14 alkyl glycidyl ether, 1, 4-butanediol diglycidyl ether and 1, 6-hexanediol diglycidyl ether;
the defoaming agent is foam-breaking polysiloxane or polymer defoaming agent without organosilicon;
the adhesion promoter is one or more of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma-aminopropyl triethoxy silane and gamma-methacryloxypropyl trimethoxy silane;
the acid donor is II type ammonium polyphosphate with polymerization degree more than 1000;
the inorganic nano-filler is one or a mixture of more than two of nano rutile type titanium dioxide, nano zinc oxide, nano aluminum hydroxide and nano magnesium hydroxide;
the reinforced fiber is one or a mixture of more than two of carbon fiber, carbon nano tube, aramid fiber, glass fiber and silicate fiber;
the rheological agent is one or two of liquid polyamide wax, bentonite rheological agent and fumed silica.
3. A solvent-free epoxy intumescent fire retardant coating as claimed in claim 1, characterized in that in component A, the preparation method of chlorinated paraffin-coated pentaerythritol comprises the following steps:
(1) putting chlorinated paraffin into an environment-friendly mixed solvent under the stirring condition of the rotating speed of 200-500 rpm, and stirring until the chlorinated paraffin is completely dissolved to form a chlorinated paraffin solution with the mass fraction of 10-30%;
(2) according to the mass ratio of 1 (1-5) of chlorinated paraffin to pentaerythritol, putting pentaerythritol powder into a chlorinated paraffin solution under the stirring condition of the rotating speed of 400-500 rpm, and increasing the rotating speed to 1500-2000 rpm until the mixture is uniformly stirred;
(3) rotationally evaporating the obtained mixture at 50-60 ℃, removing the mixed solvent, placing the mixture in an oven, and fully drying to obtain a chlorinated paraffin-coated pentaerythritol mixture;
(4) and grinding the chlorinated paraffin-coated pentaerythritol mixture by a ball mill until the average particle size reaches 40 mu m to obtain the micropowder-grade chlorinated paraffin-coated pentaerythritol.
4. The solvent-free epoxy intumescent fire retardant coating as claimed in claim 3, characterized in that the environment-friendly mixed solvent is propylene glycol butyl ether and dearomatized hydrocarbon solvent oil with a mass ratio of 1: 1.
5. The solvent-free epoxy intumescent fire retardant coating as claimed in claim 3, wherein the chlorinated paraffin is one or a mixture of more than two of chlorinated paraffins with chlorine content of 38-42 wt%, 48-52 wt% and 68-72 wt%.
6. A solvent-free epoxy intumescent fire retardant coating according to claim 3, characterized in that pentaerythritol is monopentaerythritol with a maximum particle size of 40 μm.
7. The solvent-free epoxy intumescent fire retardant coating as claimed in claim 1, wherein in the component B, the epoxy curing agent is one or a mixture of more than two of modified polyamide, modified alicyclic amine and polyether amine, and the epoxy curing agent 1, the epoxy curing agent 2 and the epoxy curing agent 3 are respectively selected from different epoxy curing agents.
8. A process for the preparation of a solventless epoxy intumescent fire retardant coating according to any one of claims 1 to 7, characterized in that it is carried out in the following sequence and steps:
the component A comprises:
(1) placing epoxy resin and a diluent in a dispersion tank, adding a defoaming agent and an adhesion promoter at the rotating speed of 500-800 rpm, and dispersing for 5-10 minutes;
(2) placing chlorinated paraffin-coated pentaerythritol, an acid donor, inorganic nano-filler, reinforcing fiber and a rheological agent in a dispersion tank in sequence, adjusting the dispersion speed to 1800-2000 rpm, starting a water bath cooling device, ensuring that the temperature of the material is lower than 60 ℃, and dispersing for 30-40 minutes;
and B component: the curing agent is mixed and dispersed for 5 to 10 minutes at a rotating speed of 200 to 300 rpm.
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| CN116004082A (en) * | 2022-12-30 | 2023-04-25 | 李�瑞 | Light solvent-free epoxy intumescent fire retardant coating for automobile power battery packs and energy storage equipment and preparation method thereof |
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| CN108264823A (en) * | 2018-02-25 | 2018-07-10 | 李嘉顺 | A kind of solvent-free thick coated type epoxy resin fireproof coating and preparation method thereof |
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| CN108264823A (en) * | 2018-02-25 | 2018-07-10 | 李嘉顺 | A kind of solvent-free thick coated type epoxy resin fireproof coating and preparation method thereof |
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