CN115418159B - Polyimide waterborne polyurethane coating and preparation method and application thereof - Google Patents
Polyimide waterborne polyurethane coating and preparation method and application thereof Download PDFInfo
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- CN115418159B CN115418159B CN202211148778.8A CN202211148778A CN115418159B CN 115418159 B CN115418159 B CN 115418159B CN 202211148778 A CN202211148778 A CN 202211148778A CN 115418159 B CN115418159 B CN 115418159B
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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
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G71/00—Macromolecular compounds obtained by reactions forming a ureide or urethane link, otherwise, than from isocyanate radicals in the main chain of the macromolecule
- C08G71/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
Abstract
The invention belongs to the technical field of aqueous polyurethane coating. The invention provides a polyimide waterborne polyurethane coating. The coating comprises 10 to 15 parts of aqueous polyimide resin, 45 to 65 parts of aqueous polyurethane resin, 5 to 10 parts of curing agent, 0.5 to 2 parts of leveling agent, 0.5 to 1 part of dispersing agent, 0.1 to 0.5 part of defoaming agent, 10 to 20 parts of pigment, 50 to 100 parts of filler and 50 to 100 parts of water. The invention also provides a preparation method and application of the polyimide waterborne polyurethane coating. The polyimide waterborne polyurethane coating disclosed by the invention has the advantages of good stability, high water resistance, low curing temperature, short curing time, environment friendliness, no toxicity, low requirements on use environment and convenience in use.
Description
Technical Field
The invention relates to the technical field of waterborne polyurethane coating, in particular to a polyimide waterborne polyurethane coating as well as a preparation method and application thereof.
Background
Polyurethane is a material obtained by addition polymerization of isocyanate and polyether. At present, a large number of different varieties and polyurethane coating systems with more outstanding quality have been formed. The waterproof coating has the advantages of good waterproof effect, high resistance, strong ground grabbing force, high flexibility, excellent high and low temperature tolerance, high corrosion resistance, convenient maintenance and the like, is highly valued and favored by the waterproof industry, is widely applied to construction of underground tunnels, roofs, subways, dams, pipelines, dense underground water layers and other projects, and is the waterproof coating most widely used and consumed.
In recent years, although the use of polyurethane coatings containing solvents and organic fillers to promote hydration of polyurethane coatings has been widely used, this has severely limited environmental awareness and concerns about health itself, as well as stringent requirements of environmental regulations for Volatile Organic Compounds (VOCs) emissions and hazardous solvent levels-powder development and high solids content.
The waterborne polyurethane is safer in use and does not volatilize a large amount of toxic and harmful gases polluting the environment, so the waterborne polyurethane becomes a hot spot in the coating world in recent years. However, compared with the traditional solvent polyurethane coating, the polyurethane coating has poor water resistance, low mechanical strength, and insufficient ageing resistance and thermal stability.
Therefore, the research and development of the water-based polyurethane coating with good water resistance, good ageing resistance, strong thermal stability and high mechanical strength has good prospect.
Disclosure of Invention
The invention aims to provide a polyimide waterborne polyurethane coating, a preparation method and application thereof, aiming at the defects of the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a polyimide waterborne polyurethane coating which comprises the following components in parts by weight:
10 to 15 parts of aqueous polyimide resin, 45 to 65 parts of aqueous polyurethane resin, 5 to 10 parts of curing agent, 0.5 to 2 parts of leveling agent, 0.5 to 1 part of dispersing agent, 0.1 to 0.5 part of defoaming agent, 10 to 20 parts of pigment, 50 to 100 parts of filler and 50 to 100 parts of water.
Preferably, the preparation method of the aqueous polyurethane resin comprises the following steps:
1) Reacting 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone with 3, 5-dihydroxybenzoic acid under the condition of concentrated sulfuric acid to obtain a product 1;
2) Reacting carbamic acid with the product 1 to obtain a product 2;
3) Reacting 4-hydroxyphthalic acid with the product 2 under dicyclohexylcarbodiimide conditions to obtain a product 3;
4) And (3) reacting the 4-hydroxy benzenesulfonic acid with the product 3 to obtain the aqueous polyurethane resin.
Preferably, the mass of the concentrated sulfuric acid in the step 1) accounts for 1-3% of the total mass of the 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone and the 3, 5-dihydroxybenzoic acid; the molar ratio of the 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone, 3, 5-dihydroxybenzoic acid, carbamic acid, 4-hydroxyphthalic acid, dicyclohexylcarbodiimide and 4-hydroxybenzenesulfonic acid is 2-20: 2-20: 3 to 21:0.5 to 2:0.05 to 0.2:0.5 to 2; the temperature of the reaction in the step 1) to the step 4) is independently 120-160 ℃, and the reaction time is independently 1-2 h.
Preferably, the structural formula of the aqueous polyurethane resin is:
wherein n is any natural number from 2 to 20.
Preferably, the curing agent is one or more of triglycidyl isocyanurate, polyisocyanate, m-xylylenediamine and isophorone diamine; the leveling agent is one or more of polydimethylsiloxane, diacetone alcohol, polyacrylate and nitrocellulose.
Preferably, the dispersing agent is one or more of sulfated castor oil, polyethylene glycol alkyl aryl ether sodium sulfonate and sulfate;
the defoaming agent is polyether defoaming agent;
the pigment is one or more of titanium dioxide, cadmium red, molybdenum-chromium orange, chromium oxide green, phthalocyanine blue and iron black;
the filler is one or more of calcium carbonate, barite powder, talcum powder, kaolin, white carbon black, mica powder and bentonite.
The invention provides a preparation method of a polyimide waterborne polyurethane coating, which comprises the following steps:
1) Mixing water-based polyimide resin, water-based polyurethane resin, a leveling agent, a dispersing agent, a part of defoaming agent and a first part of water, and then reacting to obtain a mixture I;
2) Mixing the mixture I, pigment, filler, residual defoaming agent and a second part of water, and grinding to obtain a mixture II;
3) And mixing the mixture II, the curing agent and the residual water to obtain the polyimide waterborne polyurethane coating.
Preferably, the mixing time in the step 1) is 1-2 hours, the reaction temperature is 110-130 ℃, and the reaction time is 1-2 hours; the grinding time of the step 2) is 1-3 h; the mixing time in the step 3) is 5-10 min, and the mixing rotating speed is 600-800 r/min.
Preferably, the mass ratio of the first part of water in the step 1), the second part of water in the step 2) and the residual water in the step 3) is 1-3: 3 to 5:1 to 3; the mass ratio of the part of defoaming agent in the step 1) to the rest of defoaming agent in the step 2) is 1-2: 2 to 3.
The invention also provides application of the polyimide waterborne polyurethane coating, which is prepared by mixing the polyimide waterborne polyurethane coating with water and then coating;
the mass ratio of the polyimide waterborne polyurethane coating to the water is 2-4: 1, a step of; the coating is carried out twice, and the second coating is carried out after the first coating is finished for 10-25 min.
The beneficial effects of the invention include the following points:
1) The benzenesulfonic acid group contained in the aqueous polyurethane resin can promote the self-emulsification of the polyurethane resin, and the aqueous polyurethane resin can be ground into color paste together with pigment, so that the aqueous polyurethane resin has better paint making performance compared with the additional emulsion type polyurethane resin; in addition, the self-emulsifying polyurethane emulsion is more stable, is not easy to break emulsion under the high temperature condition, does not need special equipment after the emulsion is settled, can be dispersed by slightly stirring, and is convenient to use.
2) The polyimide water-based polyurethane coating of the invention is added with the imide structure with good stability and heat resistance on the basis of the polyurethane structure, and the introduction of the rigid group not only enhances the heat stability, chemical corrosion resistance and wear resistance of polyurethane, but also can form hydrogen bonds between carbonyl groups on the imide group, thereby enhancing intermolecular acting force and microphase separation, so that the mechanical property of the material is more excellent, and the water resistance is stronger.
3) The polyimide waterborne polyurethane coating contains a triazole structure, wherein the triazole structure is a plane divalent segment with very strong rigidity, and can enhance the mechanical property and mechanical property of the coating; in addition, the addition of the triazole ring can obviously improve the thermal performance of polyurethane resin, enhance the water resistance of the coating and reduce the curing time and the curing temperature of the coating.
4) The polyimide water-based polyurethane coating disclosed by the invention has the advantages of low volatility, no harm to workers during long-term storage and blending and brushing, no need of wearing a gas mask, convenience in use, time and labor saving and low requirements on use environments.
Detailed Description
The invention provides a polyimide waterborne polyurethane coating which comprises the following components in parts by weight:
10 to 15 parts of aqueous polyimide resin, 45 to 65 parts of aqueous polyurethane resin, 5 to 10 parts of curing agent, 0.5 to 2 parts of leveling agent, 0.5 to 1 part of dispersing agent, 0.1 to 0.5 part of defoaming agent, 10 to 20 parts of pigment, 50 to 100 parts of filler and 50 to 100 parts of water.
The aqueous polyimide polyurethane coating composition of the present invention contains 10 to 15 parts of an aqueous polyimide resin, preferably 11 to 14 parts, more preferably 12 to 13 parts, and even more preferably 12.5 parts.
In the present invention, the aqueous polyimide resin is preferably a PMR-II type polyimide resin.
The polyimide aqueous polyurethane coating material of the present invention contains 45 to 65 parts of an aqueous polyurethane resin, preferably 50 to 60 parts, more preferably 53 to 57 parts, and even more preferably 55 parts.
In the invention, the preparation method of the aqueous polyurethane resin comprises the following steps:
1) Reacting 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone with 3, 5-dihydroxybenzoic acid under the condition of concentrated sulfuric acid to obtain a product 1;
2) Reacting carbamic acid with the product 1 to obtain a product 2;
3) Reacting 4-hydroxyphthalic acid with the product 2 under dicyclohexylcarbodiimide conditions to obtain a product 3;
4) And (3) reacting the 4-hydroxy benzenesulfonic acid with the product 3 to obtain the aqueous polyurethane resin.
In the invention, the mass of the concentrated sulfuric acid in the step 1) accounts for 1-3% of the total mass of the 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone and the 3, 5-dihydroxybenzoic acid, and is preferably 1.5-2.5%, and more preferably 2%; the molar ratio of the 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone, 3, 5-dihydroxybenzoic acid, carbamic acid, 4-hydroxyphthalic acid, dicyclohexylcarbodiimide and 4-hydroxybenzenesulfonic acid is 2-20: 2-20: 3 to 21:0.5 to 2:0.05 to 0.2:0.5 to 2, preferably 5 to 17:5 to 17: 6-18: 0.8 to 1.7:0.08 to 0.17:0.8 to 1.7, more preferably 10 to 12:10 to 12:10 to 14:1.1 to 1.4:0.11 to 0.14:1.1 to 1.4, more preferably 11:11:12:1.2:0.12:1.2; the temperature of the reaction in the steps 1) to 4) is independently 120-160 ℃, preferably 130-150 ℃, more preferably 135-145 ℃, and even more preferably 140 ℃; the reaction time is independently 1 to 2 hours, preferably 1.2 to 1.8 hours, more preferably 1.4 to 1.6 hours, and still more preferably 1.5 hours.
In the present invention, the concentrated sulfuric acid is preferably 98% by mass.
In the invention, the reaction equation for preparing the aqueous polyurethane resin is as follows:
wherein n is a natural number of 2 to 20, preferably 8 to 14, and more preferably 10 to 12.
The polyimide aqueous polyurethane coating composition of the present invention contains 5 to 10 parts of a curing agent, preferably 6 to 9 parts, more preferably 7 to 8 parts, and even more preferably 7.5 parts.
In the invention, the curing agent is one or more of triglycidyl isocyanurate, polyisocyanate, m-xylylenediamine and isophorone diamine, preferably triglycidyl isocyanurate, polyisocyanate or m-xylylenediamine, and more preferably triglycidyl isocyanurate or polyisocyanate; the leveling agent is one or more of polydimethylsiloxane, diacetone alcohol, polyacrylate and nitrocellulose, preferably diacetone alcohol, polyacrylate or nitrocellulose, and more preferably diacetone alcohol or polyacrylate.
The polyimide aqueous polyurethane coating of the present invention contains 0.5 to 2 parts of a leveling agent, preferably 1 to 1.5 parts, and more preferably 1.2 to 1.3 parts.
In the invention, the leveling agent is one or more of polydimethylsiloxane, diacetone alcohol, polyacrylate and nitrocellulose, preferably polydimethylsiloxane, diacetone alcohol or polyacrylate, and more preferably polydimethylsiloxane or diacetone alcohol.
The polyimide aqueous polyurethane coating material of the present invention contains 0.5 to 1 part of a dispersant, preferably 0.6 to 0.9 part, and more preferably 0.7 to 0.8 part.
In the invention, the dispersing agent is one or more of sulfated castor oil, polyethylene glycol alkyl aryl ether sodium sulfonate and sulfate salt, preferably sulfated castor oil and/or polyethylene glycol alkyl aryl ether sodium sulfonate, and more preferably sulfated castor oil and polyethylene glycol alkyl aryl ether sodium sulfonate.
The polyimide aqueous polyurethane coating material of the present invention contains 0.1 to 0.5 part of an antifoaming agent, preferably 0.2 to 0.4 part, and more preferably 0.3 part.
In the invention, the defoamer is polyether defoamer, preferably GP330 glycerin polyether defoamer and polyoxypropylene polyoxyethylene glycerin ether GPE-3000.
The aqueous polyurethane polyimide coating composition of the present invention contains 10 to 20 parts of pigment, preferably 12 to 18 parts, more preferably 14 to 16 parts, and even more preferably 15 parts.
In the invention, the pigment is one or more of titanium white, cadmium red, molybdenum-chromium orange, chromium oxide green, phthalocyanine blue and iron black, and is preferably one or more of titanium white, cadmium red, molybdenum-chromium orange and chromium oxide green.
The polyimide aqueous polyurethane coating material of the present invention contains 50 to 100 parts of filler, preferably 60 to 90 parts, more preferably 70 to 80 parts, and even more preferably 75 parts.
In the invention, the filler is one or more of calcium carbonate, barite powder, talcum powder, kaolin, white carbon black, mica powder and bentonite, and is preferably calcium carbonate, barite powder, talcum powder or kaolin.
The polyimide aqueous polyurethane coating material of the present invention contains 50 to 100 parts of water, preferably 60 to 90 parts, more preferably 70 to 80 parts, and even more preferably 75 parts.
The invention provides a preparation method of a polyimide waterborne polyurethane coating, which comprises the following steps:
1) Mixing water-based polyimide resin, water-based polyurethane resin, a leveling agent, a dispersing agent, a part of defoaming agent and a first part of water, and then reacting to obtain a mixture I;
2) Mixing the mixture I, pigment, filler, residual defoaming agent and a second part of water, and grinding to obtain a mixture II;
3) And mixing the mixture II, the curing agent and the residual water to obtain the polyimide waterborne polyurethane coating.
In the present invention, the mixing time in step 1) is 1 to 2 hours, preferably 1.2 to 1.8 hours, more preferably 1.4 to 1.6 hours, and still more preferably 1.5 hours; the reaction temperature is 110-130 ℃, preferably 115-125 ℃, and more preferably 120 ℃; the reaction time is 1 to 2 hours, preferably 1.2 to 1.8 hours, more preferably 1.4 to 1.6 hours, and still more preferably 1.5 hours; the grinding time in the step 2) is 1 to 3 hours, preferably 1.5 to 2.5 hours, more preferably 1.8 to 2.2 hours, and still more preferably 2 hours; the mixing time in the step 3) is 5-10 min, preferably 6-9 min, and more preferably 7-8 min; the rotation speed of the mixing is 600 to 800r/min, preferably 650 to 750r/min, more preferably 680 to 720r/min, and still more preferably 700r/min.
In the invention, the mass ratio of the first part of water in the step 1), the second part of water in the step 2) and the residual water in the step 3) is 1-3: 3 to 5:1 to 3, preferably 1.5 to 2.5:3.5 to 4.5:1.5 to 2.5, more preferably 2:4:2; the mass ratio of the part of defoaming agent in the step 1) to the rest of defoaming agent in the step 2) is 1-2: 2 to 3, preferably 1.2 to 1.8:2.2 to 2.8, more preferably 1.4 to 1.6:2.4 to 2.6.
The invention also provides application of the polyimide waterborne polyurethane coating, which is prepared by mixing the polyimide waterborne polyurethane coating with water and then coating;
the mass ratio of the polyimide waterborne polyurethane coating to the water is 2-4: 1, preferably 2.5 to 3.5:1, further preferably 3:1, a step of; the coating is performed in two times, and the second coating is performed for 10 to 25 minutes, preferably 15 to 20 minutes, and more preferably 18 minutes after the first coating is completed.
In the present invention, the surface of the object to be coated needs to be pretreated before the coating.
The pretreatment is a process of removing floating dust and rust on the surface of the coated object to enable the surface of the coated object to be basically flat.
In the invention, the pretreatment is followed by washing and drying; the washing adopts clear water for washing; the temperature of the drying is 80-150 ℃, preferably 100-130 ℃, further preferably 110-120 ℃, and further preferably 115 ℃; the drying time is 10 to 20 minutes, preferably 12 to 18 minutes, more preferably 14 to 16 minutes, and even more preferably 15 minutes.
In the present invention, the coating means is preferably brush coating.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
17g of 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone and 30.8g of 3, 5-dihydroxybenzoic acid are reacted for 1H under the conditions of 0.478g of concentrated sulfuric acid with the mass concentration of 98 percent and the temperature of 120 ℃ to obtain a product 1; 41.6g of carbamic acid and the product 1 are reacted for 2 hours at 130 ℃ to obtain the product 2; 9.1g of 4-hydroxyphthalic acid and the product 2 are reacted for 1h under the condition of 1.03g of dicyclohexylcarbodiimide and the temperature of 130 ℃ to obtain a product 3; 8.7g of 4-hydroxy benzene sulfonic acid and the product 3 are reacted for 2 hours at 140 ℃ to obtain the water-based polyurethane resin with n of 2.
10g of PMR-II type polyimide resin, 45g of aqueous polyurethane resin, 0.5g of polydimethylsiloxane, 0.5g of diacetone alcohol, 1g of sulfated castor oil, 0.1g of GP330 glycerol polyether defoamer and 20g of water are mixed for 1h, and then reacted for 1h at 110 ℃ to obtain a mixture I; mixing and grinding mixture I, 5g of titanium dioxide, 10g of cadmium red, 5g of molybdenum-chromium orange, 50g of talcum powder, 20g of mica powder, 20g of bentonite, 10g of barite powder, 0.2g of GP330 glycerol polyether defoamer and 60g of water for 1h to obtain mixture II; and mixing the mixture II, 5g of m-xylylenediamine and 20g of water for 5min at the rotating speed of 600r/min to obtain the polyimide waterborne polyurethane coating.
Removing floating dust and rust on the surface of a coated object, washing the surface of the coated object with clear water after the surface is basically leveled, and drying the coated object in an oven at 80 ℃ for 10min; 2g of polyimide aqueous polyurethane paint and 1g of water are mixed and then brushed on the surface of a coated object, and a second brushing is carried out after 10 min.
Example 2
25.5g of 1, 2-dihydro-3H-1, 2, 4-triazol-3-one and 46.2g of 3, 5-dihydroxybenzoic acid are reacted for 1.5H under the conditions of 2.151g of concentrated sulfuric acid with the mass concentration of 98% and the temperature of 140 ℃ to obtain a product 1; 62.4g of carbamic acid and the product 1 are reacted for 1h at 145 ℃ to obtain the product 2; reacting 18.2g of 4-hydroxyphthalic acid with 2.06g of dicyclohexylcarbodiimide at 150℃for 2h to give 3; 17.4g of 4-hydroxy benzene sulfonic acid and the product 3 are reacted for 1h at 160 ℃ to obtain the aqueous polyurethane resin with n of 3.
15g of PMR-II type polyimide resin, 65g of aqueous polyurethane resin, 0.5g of polyacrylate, 0.2g of polyethylene glycol alkyl aryl ether sodium sulfonate, 0.3g of ammonium lauryl sulfate, 0.2g of GP330 glycerol polyether defoamer and 20g of water are mixed for 2 hours, and then reacted for 2 hours at 130 ℃ to obtain a mixture I; mixing and grinding mixture I, 5g of iron black, 3g of chromium oxide green, 2g of phthalocyanine blue, 10g of calcium carbonate, 20g of mica powder, 10g of kaolin, 10g of white carbon black, 0.3g of GP330 glycerol polyether defoamer and 40g of water for 3 hours to obtain mixture II; and mixing the mixture II, 5g triglycidyl isocyanurate, 5g isophorone diamine and 20g water for 10min at the rotating speed of 800r/min to obtain the polyimide waterborne polyurethane coating.
Removing floating dust and rust on the surface of a coated object, washing the surface of the coated object with clear water after the surface is basically leveled, and then drying the coated object in an oven at 150 ℃ for 14min; 4g of polyimide aqueous polyurethane paint and 1g of water are mixed and then brushed on the surface of a coated object, and a second brushing is carried out after 25 min.
Example 3
The aqueous polyurethane resin having n of 2 prepared in example 1 was used.
Mixing 12g of PMR-II type polyimide resin, 50g of aqueous polyurethane resin, 2g of nitrocellulose, 0.3g of sulfated castor oil, 0.5g of polyethylene glycol alkyl aryl ether sodium sulfonate, 0.025g of polyoxypropylene polyoxyethylene glycerol ether GPE-3000 and 15g of water for 1.5h, and then reacting for 1.5h at 120 ℃ to obtain a mixture I; mixing and grinding a mixture I, 5g of iron black, 10g of chromium oxide green, 10g of calcium carbonate, 25g of bentonite, 15g of mica powder, 10g of kaolin, 10g of white carbon black, 0.075g of polyoxypropylene polyoxyethylene glycerol ether GPE-3000 and 25g of water for 2 hours to obtain a mixture II; and mixing the mixture II, 3g of m-xylylenediamine, 5g of triglycidyl isocyanurate and 10g of water for 8min at the rotating speed of 700r/min to obtain the polyimide waterborne polyurethane coating.
Removing floating dust and rust on the surface of a coated object, washing the surface of the coated object with clear water after the surface is basically leveled, and drying the coated object in a drying oven at 100 ℃ for 16min; after 3g of the polyimide aqueous polyurethane paint and 1g of water are mixed, the mixture is brushed on the surface of a coated object, and after 20min, a second brushing is performed.
Comparative example 1
A commercially available high temperature resistant waterborne polyurethane coating (double lion PUCM200 polyurethane topcoat) was formulated according to the instructions and applied to the surface of the coated article by brushing as in example 1.
Comparative example 2
A commercially available aqueous polyurethane waterproof paint (model AH-1704B-2) was formulated according to the instructions and applied to the surface of the object to be coated by brushing in the manner of example 2.
The coatings of examples 1-2 and comparative examples 1-2 were tested for performance, test items and methods as follows
1. Paint film hardness: GB/T6739-2006 paint and varnish pencil method to measure paint film hardness;
2. corrosion resistance: GB/T38020.2-2019 watch case and accessory gold alloy cover layer part 2: testing purity, thickness, corrosion resistance and adhesion;
VOC: measurement of Volatile Organic Compound (VOC) release amount in GB/T37884-2019 paint;
4. high temperature stability: GB/T1735-1979 paint film heat resistance assay;
5. sag resistance: evaluation of sagging resistance of GB/T9264-2012 colored paints and varnishes;
6. water resistance: GB/T1733-1993 paint film Water resistance assay;
7. color: visual colorimetry of GB/T9761-2008 colored paint and varnish colored paint;
the results of the performance tests of the coatings of examples 1 to 2 and comparative examples 1 to 2 are shown in Table 1.
TABLE 1 Performance test results of the coatings of examples 1-2 and comparative examples 1-2
As can be seen from table 1: the polyimide aqueous polyurethane coating prepared in the examples 1-2 has various performances superior to those of the common aqueous polyurethane coating used in the comparative examples 1-2 in the market, wherein the high-temperature stability is obviously superior to that of the comparative example 2, and the water resistance is obviously superior to that of the comparative example 1.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The polyimide waterborne polyurethane coating is characterized by comprising the following components in parts by weight:
10-15 parts of aqueous polyimide resin, 45-65 parts of aqueous polyurethane resin, 5-10 parts of curing agent, 0.5-2 parts of leveling agent, 0.5-1 part of dispersing agent, 0.1-0.5 part of defoaming agent, 10-20 parts of pigment, 50-100 parts of filler and 50-100 parts of water;
the aqueous polyimide resin is PMR-II polyimide resin;
the curing agent is one or more of triglycidyl isocyanurate, m-xylylenediamine and isophorone diamine; the leveling agent is one or more of polydimethylsiloxane, diacetone alcohol, polyacrylate and nitrocellulose;
the preparation method of the aqueous polyurethane resin comprises the following steps:
1) Reacting 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone with 3, 5-dihydroxybenzoic acid under the condition of concentrated sulfuric acid to obtain a product 1;
2) Reacting carbamic acid with the product 1 to obtain a product 2;
3) Reacting 4-hydroxyphthalic acid with the product 2 under dicyclohexylcarbodiimide conditions to obtain a product 3;
4) And (3) reacting the 4-hydroxy benzenesulfonic acid with the product 3 to obtain the aqueous polyurethane resin.
2. The polyimide waterborne polyurethane coating according to claim 1, wherein the mass of the concentrated sulfuric acid in the step 1) accounts for 1-3% of the total mass of 1, 2-dihydro-3H-1, 2, 4-triazole-3-one and 3, 5-dihydroxybenzoic acid; the molar ratio of the 1, 2-dihydro-3H-1, 2, 4-triazole-3-ketone to the 3, 5-dihydroxybenzoic acid to the carbamic acid to the 4-hydroxyphthalic acid to the dicyclohexylcarbodiimide to the 4-hydroxyphenylsulfonic acid is 2-20: 2-20: 3-21: 0.5-2: 0.05-0.2: 0.5-2; the temperature of the reaction in the step 1) to the step 4) is 120-160 ℃ independently, and the reaction time is 1-2 hours independently.
3. The polyimide waterborne polyurethane coating of claim 2, wherein the structural formula of the waterborne polyurethane resin is:
wherein n is any natural number from 2 to 20.
4. The polyimide waterborne polyurethane coating according to claim 3, wherein the dispersing agent is one or more of sulfated castor oil, polyethylene glycol alkyl aryl ether sulfonate and sulfate;
the defoaming agent is polyether defoaming agent;
the pigment is one or more of titanium dioxide, cadmium red, molybdenum-chromium orange, chromium oxide green, phthalocyanine blue and iron black;
the filler is one or more of calcium carbonate, barite powder, talcum powder, kaolin, white carbon black, mica powder and bentonite.
5. The method for preparing the polyimide waterborne polyurethane coating according to any one of claims 1 to 4, which is characterized by comprising the following steps:
1) Mixing water-based polyimide resin, water-based polyurethane resin, a leveling agent, a dispersing agent, a part of defoaming agent and a first part of water, and then reacting to obtain a mixture I;
2) Mixing the mixture I, pigment, filler, residual defoaming agent and a second part of water, and grinding to obtain a mixture II;
3) And mixing the mixture II, the curing agent and the residual water to obtain the polyimide waterborne polyurethane coating.
6. The method according to claim 5, wherein the mixing time of step 1)
The reaction time is 1-2 h, the reaction temperature is 110-130 ℃, and the reaction time is 1-2 h; the grinding time of the step 2) is 1-3 h; and 3) mixing for 5-10 min, wherein the mixing rotating speed is 600-800 r/min.
7. The method of claim 6, wherein step 1) the first portion of water,
The mass ratio of the second part of water in the step 2) to the residual water in the step 3) is 1-3: 3-5: 1-3; the mass ratio of the part of defoaming agent in the step 1) to the rest of defoaming agent in the step 2) is 1-2: 2-3.
8. The use of the polyimide aqueous polyurethane coating according to any one of claims 1 to 4, wherein the polyimide aqueous polyurethane coating is coated after being mixed with water;
the mass ratio of the polyimide waterborne polyurethane coating to the water is 2-4: 1, a step of; the coating is carried out twice, and the second coating is carried out after the first coating is finished for 10-25 min.
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| US5142001A (en) * | 1991-07-17 | 1992-08-25 | Kyowa Hakko Kogyo Co., Ltd. | Polyurethane composition |
| DE10260270A1 (en) * | 2002-12-20 | 2004-07-01 | Bayer Ag | Hydrophilic polyurethane-polyurea dispersion |
| CN101108951A (en) * | 2007-08-30 | 2008-01-23 | 桂林工学院 | Aquosity bi-component polyurethane coloured paint and method of manufacturing the same |
| CN106497399A (en) * | 2016-10-31 | 2017-03-15 | 邓集叶 | A kind of mechanical wear-resistant paint and preparation method thereof |
| CN108300236A (en) * | 2017-12-29 | 2018-07-20 | 山东蓝盟防腐科技股份有限公司 | A kind of modified polyurethane paint containing raw tung oil |
| CN112500774A (en) * | 2019-09-16 | 2021-03-16 | 天津大学 | Mixed type solvent-free silicon-containing waterborne polyurethane coating and preparation method thereof |
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