CN115820098B - Light flame-retardant high-toughness coating of bi-component moisture-cured polyurethane and preparation method thereof - Google Patents
Light flame-retardant high-toughness coating of bi-component moisture-cured polyurethane and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 68
- 239000011248 coating agent Substances 0.000 title claims abstract description 65
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 60
- 239000004814 polyurethane Substances 0.000 title claims abstract description 29
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
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- 229920005989 resin Polymers 0.000 claims abstract description 22
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- 239000005056 polyisocyanate Substances 0.000 claims abstract description 17
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 17
- 150000004705 aldimines Chemical class 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 27
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- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
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- 238000004806 packaging method and process Methods 0.000 claims description 13
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- 229920000515 polycarbonate Polymers 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 8
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract description 8
- 229910019142 PO4 Inorganic materials 0.000 abstract description 8
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052794 bromium Inorganic materials 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 8
- 239000003431 cross linking reagent Substances 0.000 abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 8
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- 230000000052 comparative effect Effects 0.000 description 7
- 238000004040 coloring Methods 0.000 description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 5
- 238000005452 bending Methods 0.000 description 5
- CHUGKEQJSLOLHL-UHFFFAOYSA-N 2,2-Bis(bromomethyl)propane-1,3-diol Chemical compound OCC(CO)(CBr)CBr CHUGKEQJSLOLHL-UHFFFAOYSA-N 0.000 description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
- 238000006757 chemical reactions by type Methods 0.000 description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 description 3
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- 230000008092 positive effect Effects 0.000 description 2
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- 239000007921 spray Substances 0.000 description 2
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- QEJPOEGPNIVDMK-UHFFFAOYSA-N 3-bromo-2,2-bis(bromomethyl)propan-1-ol Chemical compound OCC(CBr)(CBr)CBr QEJPOEGPNIVDMK-UHFFFAOYSA-N 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- IXQBIOPGDNZYNA-UHFFFAOYSA-N N=C=O.N=C=O.CC1=CC=CC=C1C1=CC=CC=C1C Chemical compound N=C=O.N=C=O.CC1=CC=CC=C1C1=CC=CC=C1C IXQBIOPGDNZYNA-UHFFFAOYSA-N 0.000 description 1
- JTDWCIXOEPQECG-UHFFFAOYSA-N N=C=O.N=C=O.CCCCCC(C)(C)C Chemical compound N=C=O.N=C=O.CCCCCC(C)(C)C JTDWCIXOEPQECG-UHFFFAOYSA-N 0.000 description 1
- WYNCHZVNFNFDNH-UHFFFAOYSA-N Oxazolidine Chemical compound C1COCN1 WYNCHZVNFNFDNH-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- PZBFGYYEXUXCOF-UHFFFAOYSA-N TCEP Chemical compound OC(=O)CCP(CCC(O)=O)CCC(O)=O PZBFGYYEXUXCOF-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- XXKOQQBKBHUATC-UHFFFAOYSA-N cyclohexylmethylcyclohexane Chemical group C1CCCCC1CC1CCCCC1 XXKOQQBKBHUATC-UHFFFAOYSA-N 0.000 description 1
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 150000002513 isocyanates Chemical class 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
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- 239000001301 oxygen Substances 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- KVMPUXDNESXNOH-UHFFFAOYSA-N tris(1-chloropropan-2-yl) phosphate Chemical compound ClCC(C)OP(=O)(OC(C)CCl)OC(C)CCl KVMPUXDNESXNOH-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Polyurethanes Or Polyureas (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a light flame-retardant high-toughness coating of bi-component moisture-cured polyurethane and a preparation method thereof. The bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating consists of a component A and a component B; the component A is modified polyisocyanate prepolymer resin, and is prepared from components including aliphatic isocyanate, aromatic isocyanate, oligomer polyol, bromine-containing alcohol reactive flame retardant, hydroxyl-containing phosphate reactive flame retardant, cross-linking agent, catalyst and solvent; the component B is a curing agent and is prepared from components including an aldimine latent curing agent; the bi-component moisture cured polyurethane light flame-retardant high-strength and high-toughness coating can adopt the traditional air coating process, and the prepared coating material not only has light density and flame retardant property, but also has excellent comprehensive elastic mechanical properties.
Description
Technical Field
The invention relates to the technical field of moisture-cured polyurethane elastic protective coating, in particular to a light flame-retardant high-toughness coating of bi-component moisture-cured polyurethane and a preparation method thereof.
Background
With the development of materials, the pursuit of lightweight products is gradually increasing. The composite material and other light high-strength materials have excellent performance, and compared with the traditional metals and alloys, the composite material has the special advantages of high specific strength, high specific modulus, corrosion resistance, fatigue resistance, light weight and the like, is widely applied to the fields of aerospace and the like, and greatly reduces the weight of flight equipment. However, most of the composite materials are laminated board structure designs, the mechanical properties of the longitudinal properties are very excellent, but the transverse properties have the defect of poor resistance to external impact damage, and damage to the composite material wall board caused by impact of foreign objects is unavoidable in the processes of manufacturing, transporting, assembling, using and maintaining. These types of impacts are highly likely to cause extensive delamination damage, localized fiber breakage, and microcracking within the composite. Thereby greatly reducing the physical properties of the composite material, drastically reducing the bearing capacity and even causing accidents. Coating a high-strength and high-toughness coating material on the surface of the composite material can greatly improve the impact resistance of the composite material wallboard.
At present, most materials with impact resistance or explosion prevention function at home and abroad are polyurea elastomer materials with extremely short gel time, the curing speed is extremely high, the traditional air spray gun cannot spray, and special spraying equipment is needed. In addition, related researches report that single-component polyurea can be sprayed or brushed by air, the construction is simple and convenient, but the single-component polyurea is mainly used in the field of building waterproofing, the formed coating material has obvious comprehensive elastic mechanical property difference, the tensile strength, the elongation at break, the tearing strength and other properties of the material are mainly highlighted, and the reported researches on the aspects of combined coating hardness, bending strength, density, flame retardance and the like are less. Chinese patent CN102676039A reports that prepolymer is prepared by synthesizing polyether polyol and isocyanate monomer, and is mixed with oxazolidine latent curing agent, catalyst, color paste, auxiliary agent, powder filler and the like to prepare the latent curing type single-component polyurethane coating, and the mechanical strength obtained by the method is lower and is only within 6 MPa. Chinese patent CN111763299A discloses a high-strength single-component polyurea and a preparation method thereof, which are characterized in that aliphatic isocyanate monomers, polyalcohol, solvent, catalyst and the like are adopted to synthesize prepolymer resin, and then the prepolymer resin is uniformly mixed with superfine calcium carbonate, color paste and dioxane to prepare the single-component polyurea coating, wherein the coating material has the hardness of 95A, the tensile strength of 23MPa and the elongation of 260 percent. Chinese patent CN109280469a also discloses a high-strength single-component polyurea and a preparation method thereof, after aldimine is latent cured, a dicyclohexylmethane structure is introduced into a polyurea body structure, and the prepared single-component polyurea has excellent mechanical properties of tensile mechanical strength greater than 45MPa, elongation at break greater than 400%, tear strength greater than 130N/mm, and the like.
Those skilled in the art know that the coating material can only play a role in impact resistance and protection within a certain thickness range, but the impact resistance coating material is contradictory to the requirements of the aerospace field on light weight and weight reduction of the material, and has a lower density; in addition, polyurethane coatings are flammable materials, and in order to ensure safe usability of the aircraft, the coating materials themselves are required to have good flame retardant properties.
Therefore, development of a coating with convenient spraying, excellent mechanical properties and good flame retardant property is needed at present.
Disclosure of Invention
The invention provides a light flame-retardant high-toughness coating of bi-component moisture-cured polyurethane and a preparation method thereof, aiming at solving the problems in the prior art. The bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating consists of a component A and a component B; the component A is modified polyisocyanate prepolymer resin, and is prepared from components including aliphatic isocyanate, aromatic isocyanate, oligomer polyol, bromine-containing alcohol reactive flame retardant, hydroxyl-containing phosphate reactive flame retardant, cross-linking agent, catalyst and solvent; the component B is a curing agent and is prepared from components including an aldimine latent curing agent; the bi-component moisture cured polyurethane light flame-retardant high-toughness coating can adopt a traditional air coating process, has a coating pot life of 6 hours and a surface drying time of 5-15 minutes, and the prepared coating material not only has light density and flame retardant property, but also has excellent comprehensive elastic mechanical properties, about 70D of hardness, more than 18MPa of flexural strength, more than 40MPa of tensile strength, more than 200% of elongation at break and more than 160kN/m of tear strength.
The invention aims to provide a light flame-retardant high-toughness coating of two-component moisture-cured polyurethane.
The light flame-retardant high-toughness coating consists of a component A and a component B;
the component A is modified polyisocyanate prepolymer resin, and is prepared from components including aliphatic isocyanate, aromatic isocyanate, oligomer polyol, bromine-containing alcohol reactive flame retardant, hydroxyl-containing phosphate reactive flame retardant, cross-linking agent, catalyst and solvent;
the components are calculated according to the weight portions,
the NCO content of the modified polyisocyanate prepolymer resin is 4-8%, and the solid content is 75-85%;
the component B is a curing agent and is prepared from components including an aldimine latent curing agent;
based on 100 parts by weight of aliphatic isocyanate,
70-120 parts by weight of aldimine latent curing agent; preferably 72 to 117 parts by weight;
the weight ratio of the component A to the component B is 100:10 to 20, preferably 100: 12-17.
In a preferred embodiment of the present invention,
a coloring filler can be added into the component B;
based on 100 parts by weight of aliphatic isocyanate,
0.1 to 8 parts by weight of a coloring filler; preferably 0.1 to 6 parts by weight.
In a preferred embodiment of the present invention,
the aliphatic isocyanate is at least one of isophorone diisocyanate, 4 '-dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, trimethylhexane diisocyanate and methylcyclohexyl diisocyanate, preferably at least one of isophorone diisocyanate and 4,4' -dicyclohexylmethane diisocyanate, and the main component is more than or equal to 99%; and/or the number of the groups of groups,
the aromatic isocyanate is at least one of diphenylmethane diisocyanate, toluene diisocyanate, xylylene diisocyanate and 3,3 '-dimethyl-4, 4' -biphenyl diisocyanate, preferably at least one of diphenylmethane diisocyanate and toluene diisocyanate; the aromatic isocyanate contains benzene rings which are electron-withdrawing groups and alkyl groups which are electron-pushing groups, so that the activity of the aromatic isocyanate is much higher than that of the aliphatic isocyanate, and the high-toughness coating system has the capability of rapid film forming and curing after spraying, and the aliphatic isocyanate can enhance the stability of the coating system, prolong the pot life of the coating and adjust the reaction rate; and/or the number of the groups of groups,
the low polymer polyol is polycarbonate diol or polytetrahydrofuran diol, the number average molecular weight is 800-2000 g/mol, and the water content is less than or equal to 0.2%; and/or the number of the groups of groups,
the bromine-containing alcohol reaction type flame retardant is at least one of tribromoneopentyl alcohol, dibromoneopentyl glycol, dibromoallyl alcohol, dibromoneopentyl glycol, dibromobutene diol and tetrabromoterephthalyl alcohol; and/or the number of the groups of groups,
the hydroxyl-containing phosphate reaction type flame retardant is at least one selected from O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate, tri (dipropylene glycol) phosphite and tri (glycerol) phosphite; and/or the number of the groups of groups,
the cross-linking agent is one or more of trimethylolpropane, glycerol and neopentyl glycol; and/or the number of the groups of groups,
the catalyst is at least one of dibutyl tin dilaurate and stannous octoate; and/or the number of the groups of groups,
the solvent is at least one of dimethylbenzene, butyl acetate, ethyl acetate and propylene glycol methyl ether acetate; and/or the number of the groups of groups,
the aldimine latent curing agent has an effective component of more than or equal to 95 percent and an effective amine value of 300-450 mgKOH/g, and is preferably at least one of JZ302 produced by Guangdong Jinzheng company, shanghai jun and JH-338 produced by Guangdong Jinzheng company; and/or the number of the groups of groups,
the coloring filler is a conventional coloring filler in the art, such as: light pigments such as carbon black, phthalocyanine blue or phthalocyanine green.
The formula of the invention can be added with conventional components in the field, such as white carbon black or barium sulfate in the component A, and powder filler with flame retardant effect, such as antimony trioxide, decabromodiphenyl ether, magnesium hydroxide and the like, liquid flame retardant TCPP, TCP, TCEP and the like in the conventional dosage, and the dosage can be adjusted by technicians according to actual conditions.
The second purpose of the invention is to provide a preparation method of the light flame-retardant high-toughness coating.
The method comprises the following steps:
(1) And (3) a component A: preparation of modified polyisocyanate prepolymer resin
a. Adding aliphatic isocyanate, aromatic isocyanate and 1/3-2/3 solvent, and stirring uniformly to obtain a material 1;
b. adding a catalyst and a crosslinking agent of 1/3-2/3 into the material 1, and reacting to obtain a material 2;
c. adding a mixture of oligomer dihydric alcohol, a bromine-containing alcohol reactive flame retardant and a hydroxyl-containing phosphate reactive flame retardant into the material 2, and reacting to obtain a material 3;
d. adding the residual cross-linking agent into the material 3, cooling to below 40 ℃ after the reaction, adding the residual solvent, and uniformly stirring to obtain the modified polyisocyanate prepolymer resin;
(2) And the component B comprises the following components: preparation of curing agent
Mixing the components in the component B according to the dosage ratio to obtain the curing agent;
(3) And mixing the component A and the component B according to the dosage ratio to obtain the light flame-retardant high-toughness coating.
In a preferred embodiment of the present invention,
in the step b, the reaction temperature is 60-70 ℃ and the reaction time is 0.5-1 h.
In a preferred embodiment of the present invention,
in the step c, the reaction temperature is 75-85 ℃ and the reaction time is 2-4 h.
In a preferred embodiment of the present invention,
in the step d, the reaction temperature is 75-85 ℃ and the reaction time is 1-2 h.
The invention adopts the following technical scheme:
the preparation method of the modified polyisocyanate prepolymer resin preferably comprises the following steps:
a. adding aliphatic isocyanate, aromatic isocyanate and 1/3-2/3 solvent into a reactor, and stirring for 15-30 min at 30-35 ℃ to obtain a material 1.
b. After adding the catalyst into the material 1, heating to 50-60 ℃, slowly adding 1/3-2/3 of the cross-linking agent under the stirring condition, and reacting for 0.5-1 h at 60-70 ℃ after the adding to obtain the material 2.
c. Slowly adding the mixture of the oligomer dihydric alcohol and the reactive flame retardant into the material 2 under the stirring condition at the temperature of 60-70 ℃, and reacting for 2-4 hours at the temperature of 75-85 ℃ after the dripping is finished to obtain the material 3.
d. Slowly adding the rest of cross-linking agent into the material 3 under the stirring condition at 75-85 ℃, after the adding, carrying out heat preservation reaction for 1-2 h at 75-85 ℃, after the reaction is finished, cooling to below 40 ℃, adding the rest of solvent, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 4-8%, and the solid content is 75-85%. When the NCO content exceeds 8%, the formed coating becomes hard and brittle, and the elongation at break is drastically reduced; when the NCO content is lower than 4%, the viscosity of the prepared prepolymer resin is obviously increased, and the coating becomes soft, so that the hardness and the bending strength are affected.
The preparation method of the curing agent preferably comprises the following steps:
sealing and stirring the aldimine latent curing agent and the coloring filler in a container for 0.5-1 h, grinding and dispersing by a sand mill, discharging when the fineness is less than or equal to 40 mu m, and sealing and packaging to obtain the curing agent component.
The principle and the beneficial effects of the invention are as follows:
the bi-component moisture-cured polyurethane light flame-retardant high-toughness coating prepared by the method has convenient construction performance, and the prepolymer resin structure contains a certain phosphate group because of adopting the hydroxyl-containing phosphate reaction type flame retardant, so that the coating has good leveling property and defoaming capability, and no additional defoamer or leveling agent is required to be added; the application pot life reaches more than 4 hours, the traditional air spraying can be adopted, the surface drying time is 5-15 minutes, and the actual drying time is 1-2 hours.
The polyurethane high-strength and high-toughness coating material prepared by the invention has the advantages of high hardness (Shore hardness: 68-72D), low coating density (1.05-1.20 g/cm < 3 >), high flame retardant property (oxygen index: 23-25%), high bending strength (22-27 MPa), excellent tensile strength (35-56 MPa), high elongation at break (220-270%), excellent tearing strength (160-210 kN/m) and the like.
The polyurethane high-strength and toughness coating material prepared by the invention does not contain or only contains a very small amount of coloring filler, does not contain flatting agent, defoamer and pigment filler with toughening and reinforcing functions or other functions.
According to the invention, the bromine-containing alcohol reactive flame retardant is adopted, and the flame retardant group is grafted into a part of the prepolymer resin body structure in a chemical bonding mode, so that excellent flame retardance is provided for the coating material, and more beneficial effects are achieved, namely, under the condition that the tensile strength, the elongation at break, the tearing strength and other elastic properties of the coating material are maintained, the surface hardness and the bending resistance of the coating material are greatly improved, the excellent impact resistance of the coating material is provided, and the problems of insufficient hardness of the coating material caused by adding the liquid flame retardant and rapid decrease of the elongation at break or large increase of the density of the coating material caused by adding the powder flame retardant are overcome.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The starting materials used in the examples were all conventional commercially available.
Example 1
The formula composition and the preparation process of the two-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating in the embodiment are as follows:
(1) The synthesis of the component A of the polyurethane light flame-retardant high-strength and high-toughness coating comprises the following steps:
a. 100 parts by weight of isophorone diisocyanate, 206 parts by weight of MDI-50 and 118 parts by weight of butyl acetate were added to the reactor and stirred at 35℃for 15min to give material 1.
b. After 0.29 parts by weight of dibutyltin dilaurate was added to the material 1, the mixture was heated to 60℃and 6 parts by weight of trimethylolpropane was slowly added under stirring, and after the addition, the mixture was reacted at 70℃for 0.5 hour to obtain a material 2.
c. To the material 2, 294 parts by weight of polytetrahydrofuran diol having a molecular weight of 800, 82.5 parts by weight of dibromo neopentyl glycol and 17.5 parts by weight of tris (dipropylene glycol) phosphite were slowly added under stirring at 70℃to obtain a material 3 when the reaction was carried out at 85℃for 2 hours after the completion of the dropwise addition.
d. And slowly adding 6 parts by weight of trimethylolpropane into the material 3 under the condition of stirring at the temperature of 85 ℃, carrying out heat preservation reaction for 1h at the temperature of 85 ℃ after the addition, cooling to the temperature of below 40 ℃ after the reaction is finished, adding 79 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 4.0% and the solid content is 75.0%.
(2) And (3) preparation of a component B:
114 parts by weight of JZ302 aldimine latent curing agent produced by Guangdong, jing, inc., are discharged and sealed and packaged to obtain the curing agent component.
(3) The component A and the component B prepared by the method are prepared into the bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating according to the weight ratio of A to B=100 to 12.
Example 2
The formula composition and the preparation process of the two-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating in the embodiment are as follows:
(1) The synthesis of the component A of the polyurethane light flame-retardant high-strength and high-toughness coating comprises the following steps:
a. 100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate, 206 parts by weight of TDI-80 and 49 parts by weight of butyl acetate were charged into the reactor and stirred at 30℃for 30 minutes to give a material 1.
b. After 0.29 parts by weight of dibutyltin dilaurate was added to the material 1, the mixture was heated to 50℃and under stirring, 11.75 parts by weight of trimethylolpropane was slowly added, and after the addition, the mixture was reacted at 60℃for 1 hour to obtain a material 2.
c. To the material 2, 353 parts by weight of polytetrahydrofuran diol having a molecular weight of 1000, 82.5 parts by weight of dibromo neopentyl glycol and 35 parts by weight of tris (dipropylene glycol) phosphite were slowly added under stirring at 60℃to obtain a material 3 when the reaction was carried out at 75℃for 4 hours after the completion of the dropwise addition.
d. And slowly adding 11.75 parts by weight of trimethylolpropane into the material 3 under the condition of stirring at the temperature of 75 ℃, carrying out heat preservation reaction for 2 hours at the temperature of 75 ℃, cooling to the temperature of below 40 ℃ after the reaction is finished, adding 98 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 5.2% and the solid content is 85.0%.
(2) And (3) preparation of a component B:
and (3) sealing and stirring 117 parts by weight of Shanghai jun and produced JH-338 aldimine latent curing agent and 6 parts by weight of carbon black for 0.5h in a container, grinding and dispersing by a sand mill, discharging when the fineness is less than or equal to 40 mu m, and sealing and packaging to obtain the curing agent component.
(3) The component A and the component B prepared by the method are prepared into the bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating according to the weight ratio of A to B=100 to 13.
Example 3
The formula composition and the preparation process of the two-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating in the embodiment are as follows:
(1) The synthesis of the component A of the polyurethane light flame-retardant high-strength and high-toughness coating comprises the following steps:
a. 100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate, 71.5 parts by weight of MDI-50 and 50 parts by weight of butyl acetate were charged into the reactor and stirred at 32℃for 20 minutes to give a material 1.
b. After 0.43 parts by weight of stannous octoate was added to the material 1, the mixture was heated to 55℃and 2.85 parts by weight of neopentyl glycol was slowly added under stirring, and after the addition was completed, the mixture was reacted at 70℃for 1 hour to obtain a material 2.
c. To the material 2, a mixture of 200 parts by weight of a polycarbonate diol having a molecular weight of 1000, 14.3 parts by weight of dibromobutene diol and 8.5 parts by weight of O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate was slowly added at 70℃with stirring, and after the dropwise addition, the reaction was carried out at 80℃for 3 hours to obtain a material 3.
d. Slowly adding 2.85 parts by weight of neopentyl glycol into the material 3 under the condition of stirring at 80 ℃, carrying out heat preservation reaction at 80 ℃ for 1.5 hours after the addition, cooling to below 40 ℃ after the reaction is finished, adding 50 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 7.0% and the solid content is 80.0%.
(2) And (3) preparation of a component B:
73 parts by weight of Shanghai jun and produced JH-338 aldimine latent curing agent and 2 parts by weight of carbon black are sealed and stirred for 1h in a container, and are ground and dispersed by a sand mill, and when the fineness is less than or equal to 40 mu m, the materials are discharged, sealed and packaged, so that the curing agent component is obtained.
(3) The component A and the component B prepared by the method are prepared into the bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating according to the weight ratio of A to B=100 to 15.
Example 4
The formula composition and the preparation process of the two-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating in the embodiment are as follows:
(1) The synthesis of the component A of the polyurethane light flame-retardant high-strength and high-toughness coating comprises the following steps:
a. 100 parts by weight of isophorone diisocyanate, 71.5 parts by weight of TDI-80 and 57 parts by weight of butyl acetate were added to the reactor and stirred at 32℃for 20 minutes to give material 1.
b. After 0.15 parts by weight of stannous octoate was added to the material 1, the mixture was heated to 55℃and 5.75 parts by weight of neopentyl glycol was slowly added under stirring, and after the addition was completed, the mixture was reacted at 65℃for 45 minutes to obtain a material 2.
c. To the material 2, a mixture of 200 parts by weight of a polycarbonate diol having a molecular weight of 2000, 20 parts by weight of dibromobutene diol and 17 parts by weight of O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate was slowly added at 65℃with stirring, and after the dropwise addition, the reaction was carried out at 80℃for 3 hours, to obtain a material 3.
d. Slowly adding 5.75 parts by weight of neopentyl glycol into the material 3 under the condition of stirring at 80 ℃, carrying out heat preservation reaction at 80 ℃ for 1.5 hours after the addition, cooling to below 40 ℃ after the reaction is finished, adding 57 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 8.0% and the solid content is 78.0%.
(2) And (3) preparation of a component B:
86 parts by weight of JZ302 aldimine latent curing agent produced by Guangdong, inc. and 4.5 parts by weight of carbon black are sealed and stirred for 45 minutes in a container, and are ground and dispersed by a sand mill, and when the fineness is less than or equal to 40 mu m, the materials are discharged, sealed and packaged, so that the curing agent component is obtained.
(3) The component A and the component B prepared by the method are prepared into the bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating according to the weight ratio of A to B=100 to 17.
Comparative example 1
The formulation of the paint in this comparative example was as follows:
(1) And (3) synthesizing a coating A component:
a. 100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate, 71.5 parts by weight of MDI-50 and 50 parts by weight of butyl acetate were charged into the reactor and stirred at 32℃for 20 minutes to give a material 1.
b. After 0.43 parts by weight of stannous octoate was added to the material 1, the mixture was heated to 55℃and 2.85 parts by weight of neopentyl glycol was slowly added under stirring, and after the addition was completed, the mixture was reacted at 70℃for 1 hour to obtain a material 2.
c. To the material 2, a mixture of 200 parts by weight of a polycarbonate diol having a molecular weight of 1000 and 17 parts by weight of O, O '-diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate (17 parts by weight of O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate was added to ensure 7.0% NCO%) was slowly added at 65℃with stirring, and after the dropwise addition, the reaction was carried out at 80℃for 3 hours to obtain a material 3.
d. Slowly adding 2.85 parts by weight of neopentyl glycol into the material 3 under the condition of stirring at 80 ℃, carrying out heat preservation reaction at 80 ℃ for 1.5 hours after the addition, cooling to below 40 ℃ after the reaction is finished, adding 50 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 7.0% and the solid content is 79.8%.
(2) And (3) preparation of a component B:
and (3) sealing and stirring 73 parts by weight of Shanghai jun and produced JH-338 aldimine latent curing agent and 2 parts by weight of carbon black in a container for 45min, grinding and dispersing by a sand mill, discharging when the fineness is less than or equal to 40 mu m, and sealing and packaging to obtain the curing agent component.
(3) The A component and the B component prepared by the method are prepared into the coating according to the weight ratio of A to B=100 to 15.
Comparative example 2
The formulation of the paint in this comparative example was as follows:
(1) And (3) synthesizing a coating A component:
a. 100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate, 71.5 parts by weight of MDI-50 and 50 parts by weight of butyl acetate were charged into the reactor and stirred at 32℃for 20 minutes to give a material 1.
b. After 0.43 parts by weight of stannous octoate was added to the material 1, the mixture was heated to 55℃and 2.85 parts by weight of neopentyl glycol was slowly added under stirring, and after the addition was completed, the mixture was reacted at 70℃for 1 hour to obtain a material 2.
c. To the material 2, a mixture of 200 parts by weight of a polycarbonate diol having a molecular weight of 1000 and 28.5 parts by weight of dibromobutene diol (28.5 parts by weight of dibromobutene diol was added to ensure that NCO% was 7.0%) was slowly added at 65℃under stirring, and after the completion of the dropwise addition, the reaction was carried out at 80℃for 3 hours to obtain a material 3.
d. Slowly adding 2.85 parts by weight of neopentyl glycol into the material 3 under the condition of stirring at 80 ℃, carrying out heat preservation reaction at 80 ℃ for 1.5 hours after the addition, cooling to below 40 ℃ after the reaction is finished, adding 50 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 7.0% and the solid content is 80.2%.
(2) And (3) preparation of a component B:
and (3) sealing and stirring 73 parts by weight of Shanghai jun and produced JH-338 aldimine latent curing agent and 2 parts by weight of carbon black in a container for 45min, grinding and dispersing by a sand mill, discharging when the fineness is less than or equal to 40 mu m, and sealing and packaging to obtain the curing agent component.
(3) The A component and the B component prepared by the method are prepared into the coating according to the weight ratio of A to B=100 to 15.
TABLE 1 Main Performance index of the coatings prepared in examples 1 to 4 and comparative examples 1 to 2
Examples 1 to 4 all have higher hardness, excellent flame retardant property, leveling and defoaming capability, comprehensive elastic mechanics and the like. Examples 1 to 4 have higher hardness, flexural strength and flame retardant properties than comparative example 1; examples 1 to 4 have good flame retardant properties, leveling and defoaming ability as compared with comparative example 2. In conclusion, after the bromine-containing alcohol reactive flame retardant and the hydroxyl-containing phosphate reactive flame retardant are matched, the flame retardant effect is obviously improved; wherein, the bromine-containing alcohol reactive flame retardant has positive effects on the hardness and bending resistance of the coating, and the hydroxyl-containing phosphate reactive flame retardant has positive effects on the leveling property and defoaming capability of the coating system.
Claims (2)
1. A light flame-retardant high-strength and high-toughness coating of bi-component moisture cured polyurethane is characterized in that:
the light flame-retardant high-toughness coating consists of a component A and a component B;
the component A is modified polyisocyanate prepolymer resin, and is prepared from components including 4,4 '-dicyclohexylmethane diisocyanate, MDI-50, polycarbonate diol with the molecular weight of 1000, dibromobutene diol, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate, neopentyl glycol, stannous octoate and butyl acetate;
the components are calculated according to the weight portions,
100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate;
MDI-50.5 parts by weight;
200 parts by weight of a polycarbonate diol having a molecular weight of 1000;
14.3 parts by weight of dibromobutene diol;
8.5 parts by weight of O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate;
5.7 parts by weight of neopentyl glycol;
0.43 parts by weight of stannous octoate;
100 parts by weight of butyl acetate;
the NCO content of the modified polyisocyanate prepolymer resin is 7.0% and the solid content is 80%;
the component B is a curing agent and is prepared from components including a JH-338 aldimine latent curing agent and carbon black;
73 parts by weight of JH-338 aldimine latent curing agent;
2 parts by weight of carbon black;
the weight ratio of the component A to the component B is 100: 15.
2. a method for preparing the light flame-retardant high-toughness coating according to claim 1, which is characterized in that:
the method comprises the following steps:
(1) The synthesis of the component A of the polyurethane light flame-retardant high-strength and high-toughness coating comprises the following steps:
a. adding 100 parts by weight of 4,4' -dicyclohexylmethane diisocyanate, 71.5 parts by weight of MDI-50 and 50 parts by weight of butyl acetate into a reactor, and stirring for 20min at 32 ℃ to obtain a material 1;
b. adding 0.43 part by weight of stannous octoate into the material 1, heating to 55 ℃, slowly adding 2.85 parts by weight of neopentyl glycol under the stirring condition, and reacting at 70 ℃ for 1h after the adding to obtain a material 2;
c. slowly adding a mixture of 200 parts by weight of polycarbonate diol with a molecular weight of 1000, 14.3 parts by weight of dibromobutene diol and 8.5 parts by weight of O, O' -diethyl-N, N-bis (2-hydroxyethyl) aminomethylphosphonate into a material 2 at a temperature of 70 ℃ under stirring, and reacting for 3 hours at a temperature of 80 ℃ after the dropwise addition to obtain a material 3;
d. slowly adding 2.85 parts by weight of neopentyl glycol into a material 3 under the condition of stirring at 80 ℃, after the addition, carrying out heat preservation reaction at 80 ℃ for 1.5 hours, after the reaction is finished, cooling to below 40 ℃, adding 50 parts by weight of butyl acetate, uniformly stirring, discharging, sealing and packaging to prepare the modified polyisocyanate prepolymer resin, wherein the NCO content is 7.0% and the solid content is 80.0%;
(2) And (3) preparation of a component B:
sealing and stirring 73 parts by weight of Shanghai jun and produced JH-338 aldimine latent curing agent and 2 parts by weight of carbon black for 1h in a container, grinding and dispersing by a sand mill, discharging when the fineness is less than or equal to 40 mu m, and sealing and packaging to obtain a curing agent component;
(3) The component A and the component B prepared by the method are prepared into the bi-component moisture-cured polyurethane light flame-retardant high-strength and high-toughness coating according to the weight ratio of A to B=100 to 15.
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