CN113480925A - Method for manufacturing high-performance solvent-free flame-retardant polyurea coating - Google Patents
Method for manufacturing high-performance solvent-free flame-retardant polyurea coating Download PDFInfo
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- CN113480925A CN113480925A CN202110782386.6A CN202110782386A CN113480925A CN 113480925 A CN113480925 A CN 113480925A CN 202110782386 A CN202110782386 A CN 202110782386A CN 113480925 A CN113480925 A CN 113480925A
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- polyurea coating
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- retardant
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- 229920002396 Polyurea Polymers 0.000 title claims abstract description 139
- 238000000576 coating method Methods 0.000 title claims abstract description 117
- 239000011248 coating agent Substances 0.000 title claims abstract description 112
- 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 title claims abstract description 64
- 239000003063 flame retardant Substances 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 35
- 238000003756 stirring Methods 0.000 claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- QAYVHDDEMLNVMO-UHFFFAOYSA-N 2,5-dichlorobenzene-1,4-diamine Chemical compound NC1=CC(Cl)=C(N)C=C1Cl QAYVHDDEMLNVMO-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 150000002148 esters Chemical class 0.000 claims abstract description 31
- 229920000805 Polyaspartic acid Polymers 0.000 claims abstract description 27
- 108010064470 polyaspartate Proteins 0.000 claims abstract description 27
- 239000004970 Chain extender Substances 0.000 claims abstract description 26
- 239000000049 pigment Substances 0.000 claims abstract description 23
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- 150000001412 amines Chemical group 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
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- 238000006243 chemical reaction Methods 0.000 claims description 25
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 16
- 239000002518 antifoaming agent Substances 0.000 claims description 15
- 229920005862 polyol Polymers 0.000 claims description 14
- 150000003077 polyols Chemical class 0.000 claims description 14
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 12
- RVCHQYCXJDVJQF-UHFFFAOYSA-N (3,5-diethylphenyl)methanediamine Chemical compound CCC1=CC(CC)=CC(C(N)N)=C1 RVCHQYCXJDVJQF-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 9
- QGLRLXLDMZCFBP-UHFFFAOYSA-N 1,6-diisocyanato-2,4,4-trimethylhexane Chemical compound O=C=NCC(C)CC(C)(C)CCN=C=O QGLRLXLDMZCFBP-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229920002125 Sokalan® Polymers 0.000 claims description 7
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 5
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 5
- 229930195725 Mannitol Natural products 0.000 claims description 5
- 239000000594 mannitol Substances 0.000 claims description 5
- 235000010355 mannitol Nutrition 0.000 claims description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000000600 sorbitol Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 229920000608 Polyaspartic Polymers 0.000 claims description 4
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 4
- 229960001631 carbomer Drugs 0.000 claims description 4
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 4
- -1 tetramethyl m-phenylene diisocyanate Chemical compound 0.000 claims description 4
- 229910052882 wollastonite Inorganic materials 0.000 claims description 4
- 239000010456 wollastonite Substances 0.000 claims description 4
- 239000000811 xylitol Substances 0.000 claims description 4
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 4
- 235000010447 xylitol Nutrition 0.000 claims description 4
- 229960002675 xylitol Drugs 0.000 claims description 4
- JGCWKVKYRNXTMD-UHFFFAOYSA-N bicyclo[2.2.1]heptane;isocyanic acid Chemical compound N=C=O.N=C=O.C1CC2CCC1C2 JGCWKVKYRNXTMD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000007983 Tris buffer Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 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 claims 1
- 239000005909 Kieselgur Substances 0.000 claims 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 19
- 238000005507 spraying Methods 0.000 abstract description 6
- 238000005034 decoration Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 16
- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 description 15
- 230000008569 process Effects 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
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- 238000005516 engineering process Methods 0.000 description 11
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- 239000000126 substance Substances 0.000 description 10
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- 239000011521 glass Substances 0.000 description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 229920002635 polyurethane Polymers 0.000 description 7
- 239000004814 polyurethane Substances 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
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- 239000003921 oil Substances 0.000 description 5
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- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000003973 paint Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000011083 cement mortar Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
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- 239000002689 soil Substances 0.000 description 3
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 2
- RYYWUUFWQRZTIU-UHFFFAOYSA-N Thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
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- 229940008841 1,6-hexamethylene diisocyanate Drugs 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
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Classifications
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/02—Polyureas
-
- 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
-
- 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
- C09D7/47—Levelling agents
-
- 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
- C09D7/80—Processes for incorporating ingredients
-
- 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
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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)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a manufacturing method of a high-performance solvent-free flame-retardant polyurea coating, which is characterized in that the coating consists of A, B, C three components, firstly, a component A raw material is dehydrated and prepolymerized to form a prepolymer; secondly, mixing the B component liquid amine chain extender, the polyaspartic acid ester, the 2, 5-dichloro-p-phenylenediamine and the C component anti-settling agent in a mixing kettle to form a uniform solution, and then adding the C component pigment, the flame-retardant filler and the auxiliary agent; under the condition of a certain stirring speed, the mixture becomes a mixture of the component D; then the A component prepolymer is mixed with the D component mixture and the main component in a ratio of 1: 1mol/mol to form the polyurea coating so as to complete the manufacture of the flame-retardant polyurea coating. The coating has excellent mechanical properties and performances, is simple to operate and is a novel solvent-free coating with wide application range; the coating is suitable for flame retardant protection of interior decoration of house interior walls, traffic vehicles, airplanes and ships, and is suitable for manual construction or/and spraying.
Description
The technical field is as follows:
the invention relates to a method for manufacturing a high-performance solvent-free flame-retardant polyurea coating, belonging to the field of application of high-performance coatings.
Background art:
spray polyurea elastomer technology has undergone three stages of development, polyurethane, polyurethaneurea and polyurea. In the three systems, the component A is essentially identical, and is an aromatic or aliphatic prepolymer and a semi-prepolymer, with the difference being the component B. The component B of the spray polyurethane consists of hydroxyl-terminated resin and a hydroxyl-terminated chain extender, and contains a catalyst for improving the reaction activity.
The component B of the spray polyurethane/urea can be hydroxyl-terminated resin, or can be composed of amine-terminated resin and amine chain extender, and generally contains a catalyst for improving the reaction activity. The component B of the spray polyurea is required to be composed of an amino-terminated resin and an amino-terminated chain extender, does not contain any hydroxyl component and catalyst, and can contain a certain amount of a dispersing agent and neutral ash 2 BL.
Because the reaction activity of the amino-terminated compound and the isocyanate component is extremely high, the reaction can be instantly completed at room temperature or low temperature without any catalyst, thereby effectively overcoming the fatal defects that the polyurethane and polyurethane/urea elastomer are foamed due to the influence of environmental temperature and humidity in the construction process, and the material performance is rapidly reduced.
The polyurea spraying technology integrates the advantages of anticorrosive materials such as paint, rubber, plastic and the like, and is one of the most advanced international anticorrosive technologies at present. The gel has the technical advantages that the gel is fast cured, can be sprayed on any curved surface without generating a flow phenomenon, the gel time is as short as 10s or less, and the walking strength can be achieved within 10 min; it is not sensitive to temperature and moisture, and is not influenced by ambient temperature and humidity during construction. The polyurea can be constructed in a low-temperature environment of-28 ℃ and can also be constructed in a humid and rainy environment; the paint has 100 percent of solid content, meets the requirement of environmental protection, has no smell in the construction and use processes, and is particularly suitable for the anticorrosion construction of the inner wall of a storage tank and the inner wall of a pipeline with poor ventilation; the requirement of thickness can be met by one-time construction, and the defect that the traditional anticorrosive paint needs to be constructed for many times is overcome; the coating is compact and seamless, can resist the long-term corrosion of media such as water, seawater, acid, alkali, salt, oil and the like, and has outstanding resistance to chemical media and soil erosion; the mechanical strength is high, the elongation rate is good, the impact resistance is good, and the material is not easy to damage under the action of temperature alternation and external force impact; the adhesive force is good, the adhesive force is more than 10MPa on the steel which is sand blasted to Sa2.5 grade, and the steel does not fall off after long-term use; the breakdown voltage resistance is up to more than 20kv/mm, and the matching property with cathode protection is good; the catalyst is not contained, the ultraviolet light aging resistance is good, and the paint is not pulverized and cracked after being used outdoors for a long time; wide use temperature, can be used for a long time at the temperature of between 50 ℃ below zero and 121 ℃, and the modified high temperature resistant polyurea can be used for a long time below 150 ℃, and the like.
The polyurea spraying technology has excellent physical properties and construction performance, and is a novel coating technology. The material can completely or partially replace the traditional polyurethane, epoxy resin, glass fiber reinforced plastic, FBE and polyolefin compounds, and has wide application prospect in the industries of chemical corrosion prevention, pipelines, buildings, ships, water conservancy, traffic, machinery, mine wear resistance and the like.
The anticorrosive materials for the metal chemical storage tank are generally divided into two categories, namely a lining and a coating. Commonly used liners include rubber liners, plastic liners, and glass fiber reinforced plastic liners. The rubber lining is made of natural rubber or synthetic rubber and can be used at normal temperature and pressure. The disadvantages are that the field heating vulcanization is needed, the construction process is very complicated, and the quality is difficult to ensure. The plastic lining is generally a prefabricated block material, a special pasting process is needed during construction, and leakage is easily caused at a joint, so that integral failure is caused. The glass fiber reinforced plastic lining adopts a manual pasting process, has large smell, pollutes the environment, needs a plurality of constructions and is difficult to ensure the construction quality.
The traditional anticorrosive paint has the advantage of convenient construction, and can be used on the inner wall or the outer wall. However, these coating systems generally suffer from insufficient hardness and toughness, are highly susceptible to cracking under thermal stress or impact, premature cracking can lead to leakage of stored fluids, and repair and maintenance costs are increased; the system contains organic solvent, which is harmful to human body and pollutes environment, and pinholes generated by solvent volatilization can cause penetration of corrosive medium; multiple construction is needed, the period is long, the efficiency is low, and the like.
The polyurea spraying technology effectively solves the problems, has obvious technical advantages when being applied to corrosion prevention engineering of the inner wall and the outer wall of a steel storage tank, and has been successfully applied to projects such as crude oil tanks, heavy oil tanks, sewage tanks, hydrochloric acid tank cars and the like of Daqing oil fields, Shengli oil fields, Xinjiang oil fields, Qilu petrochemical industries, Lanzhou petrochemical industries and Yueyang petrochemical industries.
In addition, the SPUA technology can also be used for chemical storage tanks with heat preservation requirements as a protective layer of a heat preservation layer. The traditional method is to wrap galvanized iron sheets outside polyurethane foam, but the existing joints are easy to cause water inflow, and the foam is quickly corroded and aged. And the adoption of the SPUA technology can play the dual roles of corrosion resistance and water resistance, has no seam, and is beautiful and practical.
In order to prevent chemical raw materials from leaking, storage tank cofferdams are built around some chemical storage tanks. Early storage tank cofferdams are simple and crude, are generally formed by enclosing concrete or concrete walls, and are paved with broken stones at the bottoms. Once a large amount of raw materials are leaked, the cofferdam can be temporarily stored, but a small amount of leaked chemical raw materials can permeate into soil to cause serious pollution to the soil. With the increasing importance of the developed countries on environmental protection, the storage tank cofferdam must be completely closed to protect the soil. The plastic lining is applied to the storage tank cofferdam and has the advantage of good corrosion resistance, but the construction process is complex, and particularly the construction is very difficult in places with complex shapes and many pipe fittings. In addition, the constructed plastic lining has a large number of seams and often causes leakage, however, the polyurea can resist the erosion of water and most chemical media and has the characteristics of no pollution, no flowing, quick construction and the like. More importantly, the polyurea elastomer after spraying has no seams, good flexibility and elongation rate of more than 300 percent, can connect the capillary cracks on the concrete substrate together, and has excellent anti-seepage effect. At present, the application of polyurea in northern western Tai and Alaska areas in foreign concrete storage tank cofferdams in large quantities indicates that polyurea can withstand severe weather tests. Besides the storage tank cofferdam, the similar application fields also include the protection of surfaces such as chemical engineering trenches, power plant drainage ditches, ground impermeable layers and the like.
Polyurea represents the current development of the international latest anticorrosion technology. Currently, many of the international well-known pipe works use polyurea or/and polyurethane foam in combination for oil and gas pipelines that need to be insulated.
With the popularization and development of the polyurea technology, the superiority of the polyurea technology is well known by people. In the near future, polyurea will become one of the main corrosion-resistant materials for the outer wall of pipes together with fusion bonded epoxy powder, 3 PE.
The SPUA material can also be widely used as the inner wall anticorrosion of nodular cast iron pipes, steel pipes and cement pipes. To achieve a service life of 50 years, the inner wall of a cast iron pipe or a steel pipe must be subjected to an anticorrosive treatment, and a cement mortar lining has been conventionally used. The cement mortar is the pipeline lining with the longest history, but is easy to crack after stress shrinkage, and has more surface defects (such as pitted surfaces, sand holes and hollows); the cement mortar lining causes the content of soluble substances to be improved, the hardness to be changed, and NH3Precipitation, leading to alkalization of the water; the instability of water also affects disadvantages of cement mortar and the like.
When CO is in water2The mortar is damaged and sand grains are lost when the over-balance concentration reaches 7mg/L, so that the water quality is influenced. The SPUA material used as an anticorrosive material for the inner wall of the cast iron pipe has the advantages of good adhesive force, no cracking, strong corrosion resistance and long service life; the surface is smooth, the hydraulic friction coefficient is less than that of a concrete pipe and a steel pipe, and the water delivery efficiency can be improved. Under the condition of the same pipe diameter, the power and the energy of the pump are saved by more than 20 percent, and the operating cost is greatly reduced; no scale formation, no pollution of water quality by bacteria microorganism in water, no secondary pollution, and no change of permanent water delivery and water quality cleanliness.
In chinese patent No: 201110101576.3 discloses a method for producing a water-soluble polyurea resin, wherein the polyurea resin obtained by the method is mainly used for coating an article. A part of polyurea resin permeates into the object, so that the adhesion between the polyurea resin and the object is improved, and the polyurea resin is mainly used for fiber coating, concrete coating, water prevention and the like. In the application process of the water-soluble polyurea, the application field is limited.
In chinese patent No: 201110403185.7, which satisfies the requirements of not requiring long-term curing, not being affected by environmental conditions when cured, and not becoming yellow upon exposure to air for a long period of time, but in fact, the curing time of the polyurea resin composition is relatively long.
In chinese patent No: 201210198415.5, the modified polyurea coating is a polyurea resin synthesized by A, B two components, and 20-50 nm zinc oxide or titanium dioxide is blended as the inorganic modified filling material of the polyurea resin, however, in the process of the invention, the granularity of the zinc oxide and titanium dioxide is increased.
Chinese patent application No: 201310132859.3 discloses a spray polyurea coating and its preparation method; in the patent, two-component raw materials are adopted to prepare the polyurea coating, and because a certain amount of various additives are required to be properly added in the preparation process of the polyurea coating, the mass ratio of various components in the raw materials of the component B is changed after the additives are added, so that obvious formula difference exists for A, B two-component polyurea coatings.
In view of the technical disadvantages of the above patents, the first object of the present invention is to provide a method for preparing a high-performance, non-solvent flame-retardant polyurea coating by a high-performance, non-polluting hand; the second purpose of the invention is to provide a manufacturing method for manufacturing a high-performance and pollution-free manual high-performance solvent-free flame-retardant polyurea coating.
The invention content is as follows:
the invention aims to research a manufacturing process of a flame-retardant polyurea coating, fully utilize the molecular structure of 2, 5-dichloro-p-phenylenediamine without increasing the manufacturing cost, improve the performance characteristics of the polyurea coating by reasonably selecting process control conditions and raw materials, achieve the final aim of optimizing the performance and simultaneously reduce the industrial production cost of the polyurea coating.
The patent researches and develops a manufacturing method of a solvent-free high-performance solvent-free flame-retardant polyurea coating, has better effect and excellent waterproof, anticorrosion and antifouling performances, and is suitable for flame-retardant protection of interior walls of houses, traffic vehicles, airplanes and ships.
The preparation method of the high-performance solvent-free flame-retardant polyurea coating is characterized in that the flame-retardant polyurea coating is composed of A, B, C components, wherein the A component is composed of isocyanate and high-functionality polyether polyol; the component B consists of 2, 5-dichloro-p-phenylenediamine, a liquid amine chain extender and polyaspartic ester; the component C consists of a filler, a pigment and an auxiliary agent, and the mole number of each component is as follows:
the component A comprises: 0.4-0.6 mol of isocyanate and 0.6-0.4 mol of high-functionality polyether polyol;
and B component: 0.1-0.3 mol of polyaspartic acid ester, 0.4-0.3 mol of 2, 5-dichloro-p-phenylenediamine and 0.5-0.4 mol of liquid chain extender;
and C, component C: 10-20 wt% of filler, 3-6 wt% of pigment, 0.5-2.5 wt% of anti-settling agent, 0.1-1.0 wt% of flatting agent and 0.01-0.3 wt% of defoaming agent;
a method for preparing a high-performance solvent-free flame-retardant polyurea coating, wherein the method for preparing the flame-retardant polyurea coating comprises the steps of dehydrating and pre-polymerizing a component A raw material into a prepolymer; secondly, mixing the B component liquid amine chain extender, the polyaspartic acid ester, the 2, 5-dichloro-p-phenylenediamine and the C component anti-settling agent in a mixing kettle to form a uniform solution, and then adding the C component pigment, the flame-retardant filler and the auxiliary agent; under the condition of a certain stirring speed, the mixture becomes a mixture of the component D; mixing the prepolymer of the component A with the mixture of the component D and the main component in a ratio of 1: 1mol/mol to form the polyurea coating so as to complete the preparation of the polyurea coating; the specific manufacturing process of the flame-retardant polyurea coating comprises the following steps:
1): adding high-functionality polyether polyol such as diethylene triamino polyether, xylitol polyether, sorbitol polyether and mannitol polyether in the component A formula into a reaction kettle, under the condition of introducing high-purity dry nitrogen, raising the temperature of a reaction kettle to 100-120 ℃, dehydrating for 2-4 h, lowering the temperature to normal temperature, adding polyisocyanates such as liquefied MDI, or/and trimethyl 1, 6-hexamethylene diisocyanate, or/and tetramethyl m-phenylene-dimethylene diisocyanate, or/and norbornane diisocyanate, or/and thiophosphoric acid tri (4-phenyl isocyanate) and the like in the formula of the component A, raising the temperature to 70-110 ℃, stirring and reacting for 2-5 h to obtain a mixture, cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): mixing polyaspartic acid ester and 3, 5-dithiotoluenediamine, or/and 3, 5-diethyltoluenediamine, or/and 3, 3 '-dichloro-4, 4' -xylene methane diamine, or/and triethylene diamine in the formula of the component B; wherein the mol ratio of 3, 5-dithiotoluenediamine, 3, 5-diethyltoluenediamine and triethylenediamine to 3, 3 '-dichloro-4, 4' -xylene methane diamine is 1: 0.6; and adding 2, 5-dichloro-p-phenylenediamine into a mixing kettle, adding 0.5-2.5 wt% of polyethylene oxide, or carbomer resin, or polyacrylic acid, or sodium polyacrylate anti-settling agent, stirring at the stirring speed of 1200-1400 rpm for 3-18 min, and then adding the rest components in the formula of the component C. Adding nanoscale wollastonite, or nanoscale barium sulfate, or nanoscale calcium sulfate, or white diatomite filler, then adding blue paste RU01, or yellow paste 6GS01, or green paste GU01, or white paste RU01 pigment, stirring for 3-9 min at the stirring speed of 600-900 rpm, then adding BYK-S706, or BYK-359, or BYK-361N flatting agent and BYK-066N, or BYK-088, or BYK-141 defoaming agent in the component C, and stirring for 2-3 min at the stirring speed of 300-600 rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) into a polyurea coating according to the mol ratio of 1: 1mol/mol, wherein the main component is isocyanate, polyether polyol, polyaspartic acid ester 2, 5-dichloro-p-phenylenediamine and liquid chain extender, and the mol ratio of the isocyanate, the polyether polyol, the polyaspartic acid ester 2, 5-dichloro-p-phenylenediamine and the liquid chain extender is 1: 1 mol/mol;
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
the mechanical properties of the preparation method of the high-performance solvent-free flame-retardant polyurea coating prepared by the method are tested by a JG/T235-2005 methodThe tensile strength is more than 45.3MPa, the elongation at break is more than 550 percent, and the tear strength is more than 73Nmm-1Limiting Oxygen Index (LOI) > 36; the energy dissipation capacity characterization adopts the sample size and the stretching rate specified in JG/T235-2005, the hysteresis curve of the sample is tested, the energy dissipation efficiency is calculated and used for characterizing the dissipation capacity, and the test result shows that the energy dissipation capacity of the manufacturing method of the high-performance solvent-free flame-retardant polyurea coating is obviously stronger than that of the current common coating.
The functional pigment is added into the resin system, so that certain properties of the coating can be effectively and pertinently improved, and the coating can be used in special environment, but the continuity of macromolecular segments is often influenced by the powder functional filler in the resin system, and the mechanical properties of the material are reduced to a certain extent. In addition, the dispersion of the powder particles in the resin often requires dilution with a large amount of solvent, which not only increases the production cost, but also causes great pollution to the environment. The invention has excellent dispersibility in a polyurea resin system without a solvent, and can construct good reflection performance and maintain good mechanical performance. The inventor formally completes the invention based on the above, and the invention provides a manufacturing method of a high-performance solvent-free flame-retardant polyurea coating, wherein the polyurea component D is formed by physically blending a heat reflection pigment and secondary amine resin, and the heat reflection pigment and the secondary amine resin react with the polyurea component A prepolymer at normal temperature to be cured into a film, and the film is dried to obtain the molded high-performance solvent-free flame-retardant polyurea coating.
In order to further improve the impact strength of the polyurea resin, in the process of the invention, 2, 5-dichloro-p-phenylenediamine and 3, 3 '-dichloro-4, 4' -xylene methane diamine are properly added, so that the strength and the flame retardance of the polyurea coating are improved, because a benzene ring structure and a-Cl flame retardant group are added in a molecular chain structure of the polyurea coating, on one hand, the rigidity of a polyurea molecular chain and the compactness of the polyurea coating are improved, the strength of the polyurea coating is improved, the integral performance characteristic of the polyurea coating is favorably improved, the limited oxygen index of the polyurea coating is increased from 21 to over 36 due to the improvement of the content of the flame retardant group, so that the polyurea coating has the flame retardance, compared with the addition of the flame retardant, the phenomenon of nonuniform dispersion of the flame retardant can be solved due to self flame retardance, and repeated experiments are carried out, it was found that with the two monomers of 2, 5-dichloro-p-phenylenediamine and 3, 3 '-dichloro-4, 4' -xylylene-methane-diamine in the molar range of the present invention, the limiting oxygen index of the polyurea coating is increased most obviously, if two monomers of 2, 5-dichloro-p-phenylenediamine and 3, 3 '-dichloro-4, 4' -xylene methane diamine are added too much, although the limited oxygen index is improved to a certain extent, the cost of the polyurea coating is obviously increased, which is not beneficial to the application and popularization of the polyurea coating, and on the contrary, the increase in the limiting oxygen index of the polyurea coating is not quite significant and, in addition, as shown by the polyurea performance characteristic data in the examples of the invention, in the process of the invention, 2, 5-dichloro-p-phenylenediamine and 3, 3 '-dichloro-4, 4' -xylene methane diamine are properly added, so that the tensile strength and the tearing strength of the polyurea coating are improved.
The manufacturing method of the high-performance solvent-free flame-retardant polyurea coating provided by the invention has excellent mechanical properties and operating performance, no additional solvent is required in the production process, the coating is completely cured when in use, no organic micromolecular harmful substance is discharged, and the coating is a novel environment-friendly coating. The filler and the pigment are added in a physical blending mode in the polyurea system, so that the color vividness of the polyurea coating is effectively improved, and meanwhile, a user can flexibly select a proper color, the production process is simple and convenient and is easy to operate, and the performance of the polyurea resin can be directly and effectively improved. Meanwhile, the manufacturing method system of the high-performance solvent-free flame-retardant polyurea coating can show excellent mechanical performance, and can resist the phenomena of coating cracking, faults, peeling and the like caused by the change of an external environment in the using process to a certain extent. The method not only avoids the use of organic solvent, saves the production cost, but also does not damage the environment, more importantly solves the problem of extremely poor mechanical property of most of the prior coatings, prolongs the service life of the coatings and widens the application field of the coatings. The preparation method of the high-performance solvent-free flame-retardant polyurea coating provided by the invention has the advantages of high strength, excellent performance, low production cost, simple manufacturing process, no environmental pollution and easiness in realizing large-scale industrial production.
In the process of the invention, the purpose of adding the leveling agent properly is to facilitate the construction of the polyurea coating, which is beneficial to the flowing of the coating no matter manual or spraying, and certainly if the addition amount of the leveling agent is too much, the polyurea coating is easy to generate the phenomenon of bead hanging in the construction process of the building outer wall, on one hand, the construction quality is affected, and on the other hand, the polyurea coating is too wasted.
In the process of the present invention, the purpose of the appropriate addition of the defoamer is to eliminate the bubbles entrained by the polyurea coating composition during agitation to reduce the bubble content in the polyurea coating while improving the compactness of the polyurea coating.
Drawings
FIG. 1 shows the performance characteristics of the high-performance solvent-free flame-retardant polyurea coating of the invention
The process flow introduction of the invention is as follows:
a method for preparing high-performance solvent-free flame-retardant polyurea coating is characterized in that the method for preparing the flame-retardant polyurea coating comprises the steps of firstly dehydrating polyether polyol in a component A raw material, carrying out prepolymerization reaction on the dehydrated polyether polyol and polyisocyanate in a formula at a certain temperature and stirring strength, and carrying out prepolymerization to obtain a prepolymer with a certain molecular weight; secondly, mixing the liquid amine chain extender, the polyaspartic acid ester, the 2, 5-dichloro-p-phenylenediamine and the 3, 3 '-dichloro-4, 4' -xylene methane diamine in the formula of the component B and the anti-settling agent in the formula of the component C in a mixing kettle to form a uniform solution, and then adding the pigment, the flame-retardant filler and various additives of the component C; under the condition of a certain stirring speed, the mixture becomes a mixture of the component D; then the A component prepolymer is mixed with the D component mixture and the main components in a ratio of 1.001: 1mol/mol to form the polyurea coating so as to complete the preparation of the flame-retardant polyurea coating.
Detailed Description
The present invention will now be described specifically by way of examples. It is to be noted that the following examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as many insubstantial modifications and variations of the invention may be made by those skilled in the art in light of the above teachings.
Example 1:
1): adding 0.6mol of diethylene triamino polyether in the formula of the component A into a reaction kettle, heating the temperature of the reaction kettle to 100 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 4 hours, cooling to normal temperature, adding 0.4mol of liquefied MDI in the formula of the component A, heating to 70-110 ℃, stirring for reacting for 2-5 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.1mol of polyaspartic acid ester, 0.5mol of 3, 5-dithiotoluenediamine and 3, 3 '-dichloro 4, 4' -xylene methane diamine in the formula of the component B; wherein the mol ratio of the 3, 5-dithiotoluenediamine to the 3, 3 '-dichloro-4, 4' -xylene methane diamine is 1: 0.6; and 0.4mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 0.5 wt% of polyethylene oxide anti-settling agent is added, stirring is carried out for 18min at the stirring speed of 1200rpm, and then the rest components in the formula of the component C are added. And adding 10 wt% of nano-wollastonite filler, then adding 3 wt% of blue paste RU01 pigment, stirring for 9min at the stirring speed of 600rpm, then adding 0.1 wt% of BYK-S706 flatting agent and 0.01 wt% of BYK-066N defoaming agent in the component C, and stirring for 3min at the stirring speed of 300rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol.
A, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Example 2:
1): adding 0.4mol of diethylene triamino polyether in the formula of the component A into a reaction kettle, heating the temperature of the reaction kettle to 120 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 2 hours, cooling to normal temperature, adding 0.6mol of trimethyl 1, 6-hexamethylene diisocyanate in the formula of the component A, heating to 110 ℃, stirring for reacting for 2 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.3mol of polyaspartic acid ester, 0.4mol of 3, 5-diethyltoluenediamine and 3, 3 '-dichloro-4, 4' -xylene methane diamine in the formula of the component B; wherein the mol ratio of 3, 5-diethyl toluenediamine to 3, 3 '-dichloro 4, 4' -xylene methane diamine is 1: 0.6; and 0.3mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 2.5 wt% of polyethylene oxide anti-settling agent is added, stirring is carried out for 18min at the stirring speed of 1400rpm, and then the rest components in the formula of the component C are added. And (2) firstly adding 20 wt% of nano-wollastonite filler, then adding 6 wt% of blue paste RU01 pigment, stirring for 3min at the stirring speed of 900rpm, then adding 1.0 wt% of BYK-S706 flatting agent and 0.3 wt% of BYK-066N defoaming agent in the component C, and stirring for 2min at the stirring speed of 600rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Example 3:
1): adding 0.5mol of xylitol polyether in the formula of the component A into a reaction kettle, heating the temperature of the reaction kettle to 105 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 3.5 hours, cooling to normal temperature, adding 0.5mol of trimethyl 1, 6-hexamethylene diisocyanate in the formula of the component A, heating to 85 ℃, stirring for reacting for 3.5 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry flame-retardant nitrogen to obtain a polyurea prepolymer of the component A;
2): 0.2mol of polyaspartic acid ester and 0.45mol of 3, 3 '-dichloro-4, 4' -xylene methane diamine in the formula of the component B; and 0.35mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 1.3 wt% of carbomer resin anti-settling agent is added, stirring is carried out for 11min at the stirring speed of 1250rpm, and then the rest components in the formula of the component C are added. And adding 13 wt% of nano barium sulfate filler, then adding 4 wt% of yellow slurry 6GS01 pigment, stirring for 5min at a stirring speed of 650rpm, adding 0.3 wt% of BYK-359 leveling agent and 0.05 wt% of BYK-088 defoaming agent in the component C, and stirring for 2.5min at a stirring speed of 400rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Comparative example 1:
1): adding 0.6mol of mannitol polyether in the formula of the component A into a reaction kettle, heating the reaction kettle to 100 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 4 hours, cooling to normal temperature, adding 0.4mol of norbornane diisocyanate in the formula of the component A, heating to 70 ℃, stirring for reacting for 5 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.1mol of polyaspartic acid ester and 0.9mol of triethylene diamine in the formula of the component B are added into a mixing kettle, 0.5 wt% of polyacrylic acid anti-settling agent is added, stirring is carried out for 18min at the stirring speed of 1200rpm, and then the rest components in the formula of the component C are added. Adding 10 wt% of nano calcium sulfate filler, then adding 3 wt% of green paste 6U01 pigment, stirring for 9min at the stirring speed of 600rpm, then adding 0.1 wt% of BYK-361N flatting agent and 0.01 wt% of BYK-141 defoaming agent in the component C, and stirring for 2min at the stirring speed of 300rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main component is isocyanate, polyether polyol, polyaspartic ester and liquid chain extender, and the mol ratio of the isocyanate to the polyether polyol to the polyaspartic ester to the liquid chain extender is 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Example 4:
adding 0.55mol of sorbitol polyether in the formula of the component A into a reaction kettle, heating the reaction kettle to 110 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 2.5 hours, cooling to normal temperature, adding 0.45mol of polyisocyanates such as thiophosphoric acid tris (4-phenyl isocyanate) and the like in the formula of the component A, heating to 90 ℃, stirring for reacting for 3.5 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.25mol of polyaspartic acid ester, 0.4mol of triethylene diamine and 3, 3 '-dichloro 4, 4' -xylene methane diamine in the formula of the component B, wherein the mol ratio of the triethylene diamine to the 3, 3 '-dichloro 4, 4' -xylene methane diamine is 1: 0.6 when the triethylene diamine and the 3, 3 '-dichloro 4, 4' -xylene methane diamine are mixed for use; and 0.35mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 2.0 wt% of carbomer resin anti-settling agent is added, the mixture is stirred for 8min at the stirring speed of 1300rpm, and then the rest components in the formula of the component C are added. Adding 16 wt% of nano calcium sulfate filler, then adding 4.5 wt% of white slurry RU01 pigment, stirring for 7min at the stirring speed of 800rpm, then adding 0.8 wt% of BYK-361N flatting agent and 0.1 wt% of BYK-088 defoaming agent in the component C, and stirring for 3min at the stirring speed of 500rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Example 5:
1): adding 0.4mol of xylitol polyether in the formula of the component A into a reaction kettle, heating the reaction kettle to 115 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 4 hours, cooling to normal temperature, adding 0.6mol of tetramethyl m-benzene-dimethylene diisocyanate in the formula of the component A, heating to 95 ℃, stirring for reacting for 5 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.2mol of polyaspartic acid ester, 0.5mol of 3, 5-diethyltoluenediamine and 3, 3 '-dichloro 4, 4' -dimethylbenzenediamine in the formula of the component B; wherein the mol ratio of 3, 5-diethyl toluenediamine to 3, 3 '-dichloro 4, 4' -xylene methane diamine is 1: 0.6; and 0.3mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 1.5 wt% of sodium polyacrylate anti-settling agent is added, stirring is carried out for 11min at the stirring speed of 1350rpm, and then the rest components in the formula of the component C are added. Adding 18 wt% of nano calcium sulfate filler, then adding 5 wt% of white slurry RU01 pigment, stirring for 3min at the stirring speed of 800rpm, then adding 0.7 wt% of BYK-359 leveling agent and 0.2 wt% of BYK-088 defoaming agent in the component C, and stirring for 2min at the stirring speed of 450rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Example 6:
adding 0.55mol of diethylene triamino polyether in the formula of the component A into a reaction kettle, heating the temperature of the reaction kettle to 100 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 2 hours, cooling to normal temperature, and adding 0.45mol of liquefied MDI and trimethyl 1, 6-hexamethylene diisocyanate in the formula of the component A, wherein the liquefied MDI: the molar ratio of trimethyl 1, 6-hexamethylene diisocyanate is 3: 1; heating to 70 ℃, stirring for reacting for 2 hours to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the flame-retardant polyurea prepolymer of the component A;
2): 0.15mol of polyaspartic acid ester, 0.45mol of 3, 5-diethyltoluenediamine and 3, 3 '-dichloro 4, 4' -dimethylbenzylmethanediamine in the formula of the component B, wherein the molar ratio of 3, 5-diethyltoluenediamine + to 3, 3 '-dichloro 4, 4' -dimethylbenzylmethanediamine is 1: 0.6 when being mixed and used, and the molar ratio of 3, 5-diethyltoluenediamine is 1: 3; and 0.4mol of 2, 5-dichloro-p-phenylenediamine is added into a mixing kettle, 1.0 wt% of sodium polyacrylate anti-settling agent is added, stirring is carried out for 18min at the stirring speed of 1400rpm, and then the rest components in the formula of the component C are added. Adding 20 wt% of nano calcium sulfate or white diatomite filler, then adding 4 wt% of green slurry GU01 pigment, stirring for 3min at the stirring speed of 600rpm, then adding 0.7 wt% of BYK-361N flatting agent and 0.2 wt% of BYK-141 defoaming agent in the component C, and stirring for 2min at the stirring speed of 500rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
Comparative example 2:
adding 0.5mol of sorbitol polyether and mannitol polyether in the component A formula into a reaction kettle, wherein the molar ratio of sorbitol polyether to mannitol polyether is 3: 2, raising the temperature of the reaction kettle to 120 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 2h, lowering the temperature to normal temperature, adding 0.5mol of trimethyl 1, 6-hexamethylene diisocyanate and tetramethyl m-benzene-dimethylene diisocyanate in the component A formula, wherein the molar ratio of methyl 1, 6-hexamethylene diisocyanate to tetramethyl m-benzene-dimethylene diisocyanate is 2: 3, raising the temperature to 110 ℃, stirring and reacting for 2h to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the component A flame-retardant polyurea prepolymer;
2): 0.1mol of polyaspartic acid ester, 0.5mol of 3, 3' -dichloro and 0.4mol of 2, 5-dichloro-p-phenylenediamine in the formula of the component B are added into a mixing kettle, 2.5 wt% of sodium polyacrylate anti-settling agent is added, stirring is carried out for 3min at the stirring speed of 1400rpm, and then the rest components in the formula of the component C are added. Adding 20 wt% of white diatomite filler, then adding 6 wt% of white slurry RU01 pigment, stirring for 3min at the stirring speed of 900rpm, then adding 1.0 wt% of BYK-361N flatting agent and 0.3 wt% of BYK-088 defoaming agent in the component C, and stirring for 2min at the stirring speed of 600rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3): mixing the main components 1) and 2) according to the proportion of 1.001: 1mol/mol to form the polyurea coating, wherein the main components comprise isocyanate, polyether glycol, polyaspartic acid ester, 2, 5-dichloro-p-phenylenediamine and liquid chain extender in a molar ratio of 1.001: 1 mol/mol;
a, D components are mixed according to the mass ratio of 1: 1.3 and coated on the surface of glass, and the polyurea coating film is obtained after drying in an oven at 50 ℃. The performance characteristics of the sheets obtained are given in the attached Table 1.
From the data of the examples 1-6 on the mass ratio of 1-2, it can be seen that the manufacturing method of the high-performance solvent-free flame-retardant polyurea coating has stronger performance, and the strength and the energy dissipation capability of the high-performance solvent-free flame-retardant polyurea coating are far stronger than those of the existing common acrylate, polyurethane and epoxy coatings.
Claims (8)
1. The preparation method of the high-performance solvent-free flame-retardant polyurea coating is characterized in that the flame-retardant polyurea coating is composed of A, B, C three components, wherein the component A is composed of isocyanate and high-functionality polyether polyol; the component B consists of 2, 5-dichloro-p-phenylenediamine, a liquid amine chain extender and polyaspartic ester; the component C consists of a filler, a pigment and an auxiliary agent, and the mole number of each component is as follows:
the component A comprises: 0.4-0.6 mol of isocyanate and 0.6-0.4 mol of high-functionality polyether polyol;
and B component: 0.1-0.3 mol of polyaspartic acid ester, 0.4-0.3 mol of 2, 5-dichloro-p-phenylenediamine and 0.5-0.4 mol of liquid chain extender;
and C, component C: 10-20 wt% of filler, 3-6 wt% of pigment, 0.5-2.5 wt% of anti-settling agent, 0.1-1.0 wt% of flatting agent and 0.01-0.3 wt% of defoaming agent.
2. The method for preparing a high-performance solvent-free flame-retardant polyurea coating according to claim 1, wherein the method for preparing the flame-retardant polyurea coating comprises the steps of dehydrating and pre-polymerizing the raw material of the component A to form a prepolymer; secondly, mixing the B component liquid amine chain extender, the polyaspartic acid ester, the 2, 5-dichloro-p-phenylenediamine and the C component anti-settling agent in a mixing kettle to form a uniform solution, and then adding the C component pigment, the flame-retardant filler and the auxiliary agent; under the condition of a certain stirring speed, the mixture becomes a mixture of the component D; mixing the prepolymer of the component A with the mixture of the component D and the main component in a ratio of 1: 1mol/mol to form the polyurea coating so as to complete the preparation of the polyurea coating; the specific manufacturing process of the flame-retardant polyurea coating comprises the following steps:
1) adding polyether polyol in the component A formula into a reaction kettle, heating the reaction kettle to 100-120 ℃ under the condition of introducing high-purity dry nitrogen, dehydrating for 2-4 h, cooling to normal temperature, adding isocyanate in the component A formula, heating to 70-110 ℃, stirring for reacting for 2-5 h to obtain a mixture, and cooling to normal temperature under the condition of introducing normal-temperature dry nitrogen to obtain the component A flame-retardant polyurea prepolymer;
2) adding polyaspartic acid ester, a liquid amine chain extender and 2, 5-dichloro-p-phenylenediamine in the formula of the component B into a mixing kettle, adding 0.5-2.5 wt% of an anti-settling agent, stirring at the stirring speed of 1200-1400 rpm for 3-18 min, and then adding the rest components in the formula of the component C; and adding the filler, then adding the pigment, stirring for 3-9 min at a stirring speed of 600-900 rpm, then adding the flatting agent and the defoaming agent in the component C, and stirring for 2-3 min at a stirring speed of 300-600 rpm to obtain a component B mixture D of the flame-retardant polyurea coating.
3) Mixing 1) and 2) main components according to the proportion of 1: 1mol/mol to form the polyurea coating, wherein the main components are isocyanate + polyether polyol: the molar ratio of the polyaspartic acid ester 2, 5-dichloro-p-phenylenediamine to the liquid chain extender is 1: 1 mol/mol.
3. The method according to claim 1, wherein the isocyanate is selected from the group consisting of liquefied MDI, trimethyl 1, 6-hexamethylene diisocyanate, tetramethyl m-phenylene diisocyanate, norbornane diisocyanate, tris (4-phenyl) thiophosphate.
4. The method according to claim 1, wherein the polyether polyol is diethylenetriaminepolyether, xylitol polyether, sorbitol polyether, or mannitol polyether.
5. The method according to claim 1, wherein the amine chain extender is selected from the group consisting of 3, 5-dithiotoluenediamine, 3, 5-diethyltoluenediamine, 3 '-dichloro-4, 4' -xylylenediamine, triethylenediamine; wherein the molar ratio of 3, 5-dithiotoluenediamine, 3, 5-diethyltoluenediamine and triethylenediamine to 3, 3 '-dichloro-4, 4' -xylylenemethanediamine is 1: 0.6.
6. The method according to claim 1, wherein the filler is selected from the group consisting of nanoscale wollastonite, nanoscale barium sulfate, nanoscale calcium sulfate, and white diatomaceous earth.
7. The method for preparing the high-performance solvent-free flame-retardant polyurea coating according to claim 1, wherein the pigment is blue paste RU01, yellow paste 6GS01, green paste GU01, white paste RU 01.
8. The method for preparing a high-performance solvent-free flame-retardant polyurea coating according to claim 1, wherein the auxiliary agent comprises an anti-settling agent, an antifoaming agent, a leveling agent, etc.; wherein the anti-settling agent is polyoxyethylene, carbomer resin, polyacrylic acid and sodium polyacrylate; the defoaming agent is high-efficiency organosilicon defoaming agent BYK-066N, BYK-088 or BYK-141; the leveling agent is BYK-S706 and BYK-359 BYK-361N.
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CN114316764A (en) * | 2022-01-06 | 2022-04-12 | 浙江吉利控股集团有限公司 | Barrier coating, preparation method thereof and method for coating barrier coating |
CN115637099A (en) * | 2022-09-29 | 2023-01-24 | 湖南大禹防水建材科技有限公司 | Solvent-free puncture-resistant polyurea waterproof coating and preparation method and application thereof |
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CN115637099A (en) * | 2022-09-29 | 2023-01-24 | 湖南大禹防水建材科技有限公司 | Solvent-free puncture-resistant polyurea waterproof coating and preparation method and application thereof |
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