CN112221754A - Metal anticorrosion nano coating and preparation method thereof - Google Patents
Metal anticorrosion nano coating and preparation method thereof Download PDFInfo
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/16—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed
- B05B7/22—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc
- B05B7/222—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas incorporating means for heating or cooling the material to be sprayed electrically, magnetically or electromagnetically, e.g. by arc using an arc
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
- B05D7/16—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies using synthetic lacquers or varnishes
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D175/06—Polyurethanes from polyesters
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a metal anticorrosion nano coating and a preparation method thereof, and the preparation method comprises the following steps: (1) uniformly mixing nano modified polyurethane resin, a thickening agent, porous powder, a synergist, an anti-rust pigment, a dispersing agent, a defoaming agent and an anti-skinning agent, adding the mixture into a ball mill at a certain temperature, and carrying out ball milling to obtain modified nano modified polyurethane finish paint; (2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating. The invention has the beneficial effects that the efficient multi-atomization electric arc spraying system is adopted, the nano modified fluorine-containing finish paint is prepared, the binding force between the finish paint and a substrate is increased through the physical hole sealing and the effect of enhancing the chemical bond binding, the coating damage is prevented, the service life of the coating is prolonged, and the purpose of preventing metal failure is effectively achieved.
Description
Technical Field
The invention relates to the field of coatings, in particular to a metal anticorrosion nano coating and a preparation method thereof.
Background
The anticorrosion coating is a covering layer which is generally coated on the surface of metal to isolate the surrounding water and air so as to prevent the metal from being corroded, and the mechanism of the anticorrosion coating is to form a shielding protective layer on the surface of the metal to prevent water and oxygen from contacting with the surface of the metal, so that the anticorrosion coating has good electrical insulation and water resistance, has strong adhesive force with the surface of the metal, can resist chemical damage and has certain mechanical strength, but a great deal of research shows that the coating always has certain air permeability and water permeability, the water and oxygen permeation speed of the coating is usually higher than the water and oxygen consumption speed of the corrosion of the surface of exposed steel, and the coating cannot achieve the complete shielding effect. The anticorrosive coating is composed of three parts, the first layer is a primer coated on the surface of the metal to enhance the bonding force between the metal and the main coating, the second layer is a finish coat, common materials comprise coal tar enamel, petroleum asphalt, polyethylene adhesive tapes, epoxy resin, polyolefin coatings and the like, and the finish coat plays an important role in metal corrosion prevention.
At most, the anticorrosion coating on the current market can realize 20 years of protection, the damage of the coating causes the protection age to be even less than 20 years, the service life of the metal material is far longer than 20 years, therefore, a better anticorrosion coating needs to be developed to improve the service life of the metal, the anticorrosion coating on the current market has weak bonding force with the metal surface, is easy to damage, has large gap between the coating and the metal, and still needs to improve the protection effect on the metal.
CN201810287336.9 discloses an anticorrosion treatment method for field construction of an elastic anticorrosion coating, belonging to the technical field of field anticorrosion construction treatment of pipelines. The technical scheme is as follows: finding the position of a metal pipeline connecting piece needing anti-corrosion treatment; secondly, wrapping the plastic heat shrinkage film on the surface of the metal pipeline connecting piece in a winding manner, heating the plastic heat shrinkage film, and completely wrapping the surface of the whole metal pipeline connecting piece after the plastic heat shrinkage film is heated and shrunk so that the metal pipeline connecting piece can obtain a relatively flat construction surface; and thirdly, spraying an elastic anti-corrosion coating on the surface of the plastic heat shrinkage film of the metal pipeline connecting piece, wherein the elastic anti-corrosion coating completely covers the plastic heat shrinkage film. The invention solves the technical problem that when the elastic anticorrosive coating is constructed on site, the rust on the surfaces of metal connecting pieces such as flanges, valves, loose joints and the like can not be completely removed by manual rust removal, so that the requirements of reactive spraying construction can not be met. The invention does not mention the problem of how to improve the binding force between the anticorrosive coating and the metal surface and improve the service life of the anticorrosive coating.
CN107892866A discloses a boron nitride anticorrosive coating material and a preparation method thereof, belonging to the field of chemical industry. The boron nitride anticorrosive coating material comprises the following components in parts by weight: water-based alkyd resin: 22-24 parts of nano boron nitride: 5-7 parts of a dispersant: 0.6-1.6 parts of solvent: 70-85 parts. The preparation method comprises the following steps: a. mixing nano boron nitride with a solvent to prepare boron nitride slurry; b. adding a dispersant into the prepared boron nitride slurry to prepare a boron nitride filler dispersion liquid; c. and mixing the prepared boron nitride filler dispersion liquid with water-based alkyd resin to prepare the boron nitride anticorrosive coating material. The preparation method of the anticorrosive coating material is simple, the coating thickness range of the prepared anticorrosive coating material is 20-25 mu m, the substrate material can be protected for 7-8 years at the high temperature of 300 ℃, and the anticorrosive coating material has excellent anticorrosive effect. The method provided by the invention has excellent anticorrosion effect, but the cost of boron nitride is high, and the boron nitride and the matrix material are not connected through chemical bonds and are easy to damage.
CN201810633023.4 discloses a steel anti-corrosion coating, which is prepared from the following raw materials in percentage by weight: 55-65% of organic silicon modified fluorine-containing film-forming resin, 2-5% of dispersing agent, 2-5% of defoaming agent and the balance of organic solvent. The invention also discloses a preparation method of the steel anti-corrosion coating, which comprises the following steps: mixing the raw materials, dispersing for 20-30min in a high-speed dispersion machine with the rotation speed of 800-. The steel anticorrosive coating disclosed by the invention has excellent anticorrosive performance, simple anticorrosive construction coating process and stable coating performance. The coating prepared by the method provided by the invention is not chemically bonded with the base material, and is easy to damage.
According to statistics, the metal loss caused by corrosion reaches hundreds of millions of yuan every year, the quality of the anticorrosive coating directly determines the service life of the metal material, and the anticorrosive coating is an indispensable part in the construction process of the metal material, so that the development of the anticorrosive coating with longer service life and better anticorrosive effect has great significance.
Disclosure of Invention
The invention provides a metal anticorrosion nano coating and a preparation method thereof, wherein a high-efficiency multi-atomization electric arc spraying system is adopted, nano modified fluorine-containing finish paint is prepared, the bonding force between the finish paint and a substrate is increased through the functions of physical hole sealing and chemical bond bonding enhancement, the damage of the coating is prevented, the service life of the coating is prolonged, and the purpose of preventing metal failure is effectively achieved. .
A metal anticorrosion nano coating and a preparation method thereof are characterized by comprising the following steps:
(1) according to the mass fraction, 50-70 parts of nano modified polyurethane resin, 15-20 parts of thickening agent, 20-30 parts of porous powder, 5-10 parts of synergist, 3-8 parts of antirust pigment, 0.5-2.0 parts of dispersing agent, 0.5-1.5 parts of defoaming agent and 0.05-0.1 part of anti-skinning agent are uniformly mixed and added in an amount of 0-10 partsoC, adding the mixture into a ball mill, and ball-milling for 2-4h at 2500-;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
Preferably, the preparation method of the nano modified polyurethane resin comprises the following steps:
according to the mass portion, 60-80 portions of polyester polyol with the number average molecular weight of 1000-4000 are heated to 110-130 ℃, vacuumized to-0.08 to-0.1 MPa, kept for 2-4h and then cooled to 45-60oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 30-40 parts of MDI (diphenylmethane diisocyanate) and 80-90 parts of MDIoC, reacting for 2-4h under the protection of nitrogen; after the reaction is finished, 3 to 8 parts of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1 to 0.5 part of stannous octoate are added, and the temperature is raised to 80 to 90oC, reacting for 30-60min, and cooling to 0-10oC, adding 80-100 parts of solvent acetone and 5-10 parts of nano titanium oxide,0.2-0.6 part of 2, 3-naphthalocyanine tin, 0.7-1.6 parts of KH-792 and 0.3-0.9 part of stearic acid monoglyceride, and the nano modified polyurethane can be obtained by high-speed shearing dispersion for 80-100min at 65-75 ℃.
The preparation method of the synergist comprises the following steps:
according to the mass portion, 15-22 portions of glyoxal and 1.2-3.3 portions of 2- (thiophene-2-yl) phenol, 1.5-4.2 portions of (R) -1, 1-spiroindane-7, 7-diphenol, 100 portions of tetrahydrofuran are evenly stirred, the pH value of the solution is adjusted to be neutral by sodium hydroxide, the solution is continuously stirred for 20-90min at 60-70 ℃, then 1-4 portions of hexamethylenetetramine are added into a reaction kettle, and the mixture is stirred for 60-180min at room temperature; then slowly heating to 65-77 ℃, stirring for 15-30min, adjusting the pH value to 3-5, and carrying out heat preservation reaction for 150-200 min; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
Preferably, the porous powder in the step (1) is one or a combination of several of nano porous alumina, mesoporous silica, nano porous boron nitride and nano porous silicon carbide;
preferably, the thickener in step (1) is one or a combination of several of nano carbon black, carbon nano tube and fumed silica;
preferably, the antirust pigment in the step (1) is one or a combination of more of red lead powder, iron red powder, composite iron titanium powder, aluminum tripolyphosphate zinc powder and zinc caseinate;
preferably, the dispersant is one or a combination of more of sodium oleate, oleyl oleate, pyridinium propanesulfonate, sodium polynaphthalenesulfonate and sodium polyacrylate;
preferably, the defoaming agent is one or a combination of more of trialkyl melamine, cyanuric chloride melamine, dialkyl phosphate and fluorinated alkyl phosphate, palmitic acid and fatty glyceride;
preferably, the anti-skinning agent is one or a combination of more of methyl ethyl ketoxime, turpentine, dipentene and butanedione monoxime;
preferably, the technological parameter of the high-efficiency multi-atomization electric arc spraying is atomization gasThe pressure is 0.6MPa, and the flow of the atomizing gas is 2.5m3And/min, the spraying voltage is 33V, the spraying angle is 74 degrees, and the spraying distance is 200 mm.
The partial reaction mechanism equation in the preparation process of the anticorrosive coating is shown as follows:
further, the glyoxal and 2- (thiophene-2-yl) phenol, (R) -1, 1-spiroindane-7, 7-diphenol are subjected to polycondensation reaction, and spiroindane and thiophene groups are introduced into the metal anticorrosion nano-coating, and the reaction formula of part of the reaction mechanism is as follows:
the invention has the beneficial effects that:
1. by adopting a high-efficiency multi-atomization arc spraying system, the obtained coating is more tightly combined with the surface of the substrate, the adhesion of the coating on the substrate is improved, and the service life of the coating is greatly prolonged;
2. the polarity of the coating is reduced, the contact angle of the coating is improved, and finally the self-cleaning capability of the coating is greatly improved by introducing the nano modified polyurethane resin into the coating substrate;
3. by introducing the nano particles into the coating, the strength of the coating is greatly improved, the wear resistance of the coating is enhanced, and the service life of the coating is prolonged;
4. the glyoxal and 2- (thiophene-2-yl) phenol, (R) -1, 1-spiroindane-7, 7-diphenol are subjected to polycondensation reaction, and the spiroindane and the thiophene are introduced into the metal anticorrosion nano coating, so that the coating and the metal surface are linked through chemical bonds, the adhesive force of the coating on the metal surface is improved, the problem of low adhesive force of the coating on the metal surface caused by adding more nano modified polyurethane resin is solved, and the anti-stripping capability of the coating is improved.
Drawings
FIG. 1 is a Fourier Infrared Spectroscopy of the product obtained in example 9:
at 1201cm-1An absorption peak of a fluorocarbon bond at 1785/1702cm is present in the vicinity-1The absorption peak of carbonyl group of amide at 1372cm-1The absorption peak of the carbon-nitrogen single bond of the amide exists nearby and is 1498cm-1An absorption peak of a benzene ring exists nearby, which indicates that the modified nano modified polyurethane resin participates in the reaction; at 494cm-1An absorption peak of silicon dioxide exists nearby, which indicates that the gas-phase silicon dioxide and the mesoporous silicon dioxide participate in the reaction; at 1603cm-1The absorption peak of carbon-nitrogen double bond is 3179cm-1An absorption peak of a nitrogen-hydrogen bond exists nearby, which indicates that the melamine formaldehyde participates in the reaction; at 896cm-1The absorption peak of phosphorus-oxygen single bond exists nearby, which indicates that the fluorinated alkyl phosphate participates in the reaction.
Detailed Description
The raw materials used in the following examples are all commercial products, wherein g is the weight g, and the examples are further illustrative of the present invention and do not limit the scope of the present invention;
the performance test methods are as follows:
1. neutral salt spray test: and (3) performing a neutral salt spray test on the anticorrosive coating according to the regulation of the national standard GB/T10125 salt spray test for artificial atmosphere corrosion test.
2. Contact angle analysis method: the sample was molded into a rectangular piece and placed in a jacket, and the contact angle of the sample film with water was measured by a dynamic surface energy analyzer of KrOssK12 type.
Example 1
(1) 50g of nano modified polyurethane resin, 15g of nano carbon black, 30g of nano porous alumina, 5g of polydimethylsiloxane, 3g of red lead powder, 0.5-2.0g of dispersing agent, 0.5g of trialkyl melamine and 0.05g of methyl ethyl ketoxime are uniformly mixed and added at 0oC, adding the mixture into a ball mill, and ball-milling for 2 hours at 2500r/min to modify the nano modified polyurethane finish;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
heating 60g of polyester polyol with the number average molecular weight of 1000 to 110 ℃, vacuumizing to-0.08 MPa, keeping for 2h, and then cooling to 45%oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 30g of MDI, 80oC, reacting for 2 hours under the protection of nitrogen; after the reaction was complete, 3g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1g of stannous octoate were added and the temperature was raised to 80%oC, reacting for 30min, and cooling to 0oAnd C, adding 80g of solvent acetone, 5g of nano titanium oxide, 0.2g of 2, 3-naphthalocyanine tin, 0.7g of KH-792 and 0.3g of stearic acid monoglyceride, and shearing at high speed at 65 ℃ for g-dispersing for 80min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 15g of glyoxal and 1.2g of 2- (thiophene-2-yl) phenol, 1.5g of (R) -1, 1-spiroindane-7, 7-diphenol and 100g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 20min at 60 ℃, then adding 1g of hexamethylenetetramine into a reaction kettle, and stirring for 60min at room temperature; then slowly heating to 65 ℃, stirring for 15min, adjusting the pH value to 3, and reacting for 150min under the condition of heat preservation; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating has the advantages of no bubbling, no rusting and no peeling after being subjected to a saline water resistance test 902h, and the contact angle is 120 degrees.
Example 2
(1) Mixing 52.8g of nano modified polyurethane resin, 15.2g of carbon nano tube, 29g of mesoporous silica, 5.7g of polymethylphenylsiloxane, 3.2g of iron oxide red powder, 0.5-2.0g of powder, 0.6g of cyanuric chloride melamine and 0g of turpentine uniformly in a proportion of 1.3goC, adding the mixture into a ball mill, and ball-milling for 2.2 hours at 2500r/min to modify the nano modified polyurethane finish;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
heating 61.1g of polyester polyol with the number average molecular weight of 1300 to 111.7 ℃, vacuumizing to-0.1 MPa, keeping for 2.2h, and then cooling to 46.6oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 31.3g of MDI, 81.1oC, reacting for 2.2 hours under the protection of nitrogen; after the reaction was complete, 3.6g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1g of stannous octoate were added and the temperature was raised to 81.3oC, reacting for 32.3min, and cooling to 1.3oC, adding 82.6g of acetone solvent, 5.6g of nano titanium oxide, 0.2g of 2, 3-naphthalocyanine tin and 0.8g of nano titanium oxideKH-792 and 0.3g of stearic acid monoglyceride are sheared at a high speed at 65.6 ℃ to g-disperse for 82.8min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 16g of glyoxal and 1.4g of 2- (thiophene-2-yl) phenol, 1.7g of (R) -1, 1-spiroindane-7, 7-diphenol and 103g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 20-90min at 62 ℃, then adding 2g of hexamethylenetetramine into a reaction kettle, and stirring for 80min at room temperature; then slowly heating to 67 ℃, stirring for 17min, adjusting the pH value to 3, and carrying out heat preservation reaction for 160 min; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating does not blister, rust and peel after a salt water resistant experiment 903h, and the contact angle is 121 degrees.
Example 3
(1) 54.3g of nano modified polyurethane resin, 15.5g of fumed silica, 28.4g of nano porous boron nitride, 6.4g of polyether modified polysiloxane, 3.7g of composite ferrotitanium powder, 0.5-2.0g of powder, 0.6g of dialkyl phosphate and 0g of dipentene are uniformly mixed, and the mixture is stirred at the speed of 2.1goC, adding the mixture into a ball mill, and ball-milling for 2.5 hours at 2500r/min to modify the nano modified polyurethane finish;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
heating 63.3g of polyester polyol with the number average molecular weight of 1500 to 112.8 ℃, vacuumizing to-0.1 MPa, keeping for 2.4h, and then cooling to 48.7oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 31.8g of MDI, 81.7 goC, reacting for 2.3 hours under the protection of nitrogen; after the reaction was complete, 3.9g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1g of stannous octoate were added, and the temperature was raised to 82.5oC, transCooling to 1.9 minoAnd C, adding 83.7g of solvent acetone, 5.9g of nano titanium oxide, 0.2g of 2, 3-naphthalocyanine tin, 0.9g of KH-792 and 0.3g of stearic acid monoglyceride, and shearing at a high speed at 67.1 ℃ to disperse for 85.2min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 19g of glyoxal and 1.7g of 2- (thiophene-2-yl) phenol, 1.9g of (R) -1, 1-spiroindane-7, 7-diphenol and 109g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 40min at 65 ℃, adding 2g of hexamethylenetetramine into a reaction kettle, and stirring for 110min at room temperature; then slowly heating to 68 ℃, stirring for 20min, adjusting the pH value to 4, and reacting for 180min under the condition of heat preservation; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating has the advantages of no bubbling, no rusting and no peeling after being subjected to a saline water resistance test 906h, and the contact angle is 122 degrees.
Example 4
(1) Mixing 55.6g nanometer modified polyurethane resin, 16.1g nanometer carbon black, 27g nanometer porous silicon carbide, 6.9g alkyl modified polysiloxane, 4g aluminium trippolyhosphate zinc powder, 0.5-2.0g dispersant, 0.7g fatty acid glyceride and 0g butanedione monoxime uniformly, and adding into a container 2.6goC, adding the mixture into a ball mill, and carrying out ball milling at 2600r/min for 2.7h to modify the nano modified polyurethane finish;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
heating 64.4g of polyester polyol with the number average molecular weight of 2100 to 114.8 ℃, vacuumizing to-0.1 MPa, keeping for 2.5h, and then cooling to 50 DEG CoC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 32.4g of MDI, 83oC, reacting for 2.4 hours under the protection of nitrogen(ii) a After the reaction was complete, 4.5g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1g of stannous octoate were added and the temperature was raised to 83.3oC, reacting for 38.3min, and cooling to 3.4oAnd C, adding 85.2g of solvent acetone, 6.6g of nano titanium oxide, 0.2g of 2, 3-naphthalocyanine tin, 0.9g of KH-792 and 0.3g of stearic acid monoglyceride, and shearing at a high speed at 68.5 ℃ for g and dispersing for 86.3min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 19g of glyoxal and 2.1g of 2- (thiophene-2-yl) phenol, 2.1g of (R) -1, 1-spiroindane-7, 7-diphenol and 112g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 70min at 67 ℃, then adding 3g of hexamethylenetetramine into a reaction kettle, and stirring for 170min at room temperature; then slowly heating to 69 ℃, stirring for 25min, adjusting the pH value to 5, and reacting for 180min under the condition of heat preservation; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating has the advantages of no bubbling, no rusting and no peeling after being subjected to a salt water resistance test 922h, and the contact angle is 122 degrees.
Example 5
(1) 65.7g of nano modified polyurethane resin, 18.1g of carbon nano tube, 22.7g of nano porous silicon carbide, 9.4g of alkyl modified polysiloxane, 6.1g of aluminum tripolyphosphate zinc powder, 0.5-2.0g of dispersing agent, 0.9g of fatty acid glyceride and 0g of butanedione monoxime are uniformly mixed in 6.2g ofoC, adding the mixture into a ball mill, and ball-milling for 3.3 hours at 2900r/min to modify the nano modified polyurethane finish paint;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
71.8g of polyester polyol with the number average molecular weight of 3200 is heated to 122.4 ℃, vacuumized to-0.1 MPa and kept for 3.2hThen cooling to 55.7oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 36.2g of MDI, 88oC, reacting for 3.2 hours under the protection of nitrogen; after the reaction was complete, 6.2g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1g of stannous octoate were added and the temperature was raised to 87.2oC, reacting for 49.5min, and cooling to 7.5oAnd C, adding 95.3g of solvent acetone, 8.1g of nano titanium oxide, 0.2g of 2, 3-naphthalocyanine tin, 1g of KH-792 and 0.3g of stearic acid monoglyceride, and shearing at high speed at 73.5 ℃ for g-dispersion for 94min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 21g of glyoxal and 3.2g of 2- (thiophene-2-yl) phenol, 3.8g of (R) -1, 1-spiroindane-7, 7-diphenol and 117g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 80min at 69 ℃, then adding 3g of hexamethylenetetramine into a reaction kettle, and stirring for 170min at room temperature; then slowly heating to 74 ℃, stirring for 28min, adjusting the pH value to 5, and carrying out heat preservation reaction for 190 min; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating has no bubbling, rust and peeling after being subjected to a salt water resistance test for 950h, and the contact angle is 126 degrees.
Example 6
(1) 70g of nano modified polyurethane resin, 20g of fumed silica, 20g of mesoporous silica, 10g of melamine formaldehyde, 8g of red lead powder, 0.5-2.0g of dispersing agent, 1.5g of fluorinated alkyl phosphate and 0.1g of butanedione monoxime are uniformly mixed, and the mixture is stirred at 10goC, adding the mixture into a ball mill, and carrying out ball milling at 3000r/min for 4h to modify the nano modified polyurethane finish;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
The preparation method of the nano modified polyurethane resin comprises the following steps:
80g of polyester polyolThe polyester polyol has the number average molecular weight of 4000, is heated to 130 ℃, is vacuumized to-0.08 MPa, is kept for 4 hours, and is cooled to 60 DEGoC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 40g of MDI, 90oC, reacting for 4 hours under the protection of nitrogen; after the reaction was complete, 8g of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.5g of stannous octoate were added and the temperature was raised to 90%oC, reacting for 60min, and cooling to 10 DEGoAnd C, adding 100g of solvent acetone, 10g of nano titanium oxide, 0.6g of 2, 3-naphthalocyanine tin, 1.6g of KH-792 and 0.9g of stearic acid monoglyceride, and shearing at a high speed at 75 ℃ for 100min to obtain the nano modified polyurethane.
The preparation method of the synergist comprises the following steps:
uniformly stirring 22g of glyoxal, 3.3g of 2- (thiophene-2-yl) phenol, 4.2g of (R) -1, 1-spiroindane-7, 7-diphenol and 120g of tetrahydrofuran, adjusting the pH value of the solution to be neutral by using sodium hydroxide, continuously stirring for 90min at 70 ℃, adding 4g of hexamethylenetetramine into a reaction kettle, and stirring for 180min at room temperature; then slowly heating to 77 ℃, stirring for 30min, adjusting the pH value to 5, and reacting for 200min under the condition of heat preservation; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
The obtained coating has no bubbling, rust and peeling after 960h of salt water resistance test, and the contact angle is 130 degrees.
Comparative example 1
The addition amount of 0g of dodecanediol relative to that of example 1, 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol produced showed no blistering, no rusting, no peeling off and a contact angle of 108 degrees in a brine resistance test of 830H.
Comparative example 2
Compared with the example 1, the content of the synergist is 0g, and the obtained coating has the advantages of no bubbling, no rusting and no peeling after the brine resistance test of 790h and a contact angle of 113 degrees.
Comparative example 3
Compared with the example 1, the content of the 2- (thiophene-2-yl) phenol is 0g, and the obtained coating does not bubble, rust and peel after being subjected to a salt water resistance test for 880h, and has a contact angle of 120 degrees.
Comparative example 4
Relative to example 1, the content of (R) -1, 1-spiroindane-7, 7-diphenol is 0g, and the obtained coating has no bubbling, rustiness and peeling after a salt water resistance test of 860h and a contact angle of 116 degrees.
Claims (10)
1. A metal anticorrosion nano coating and a preparation method thereof are characterized by comprising the following steps:
(1) according to the mass fraction, 50-70 parts of nano modified polyurethane resin, 15-20 parts of thickening agent, 20-30 parts of porous powder, 5-10 parts of synergist, 3-8 parts of antirust pigment, 0.5-2.0 parts of dispersing agent, 0.5-1.5 parts of defoaming agent and 0.05-0.1 part of anti-skinning agent are uniformly mixed and added in an amount of 0-10 partsoC, adding the mixture into a ball mill, and ball-milling for 2-4h at 2500-;
(2) and (2) carrying out sand blasting on the metal surface to remove impurities, spraying an aluminum layer on the metal surface by utilizing high-efficiency multi-atomization arc spraying, and then spraying an epoxy seal primer, an epoxy micaceous iron intermediate paint and the prepared finish paint by adopting a high-pressure airless spraying method to obtain the metal anticorrosion nano coating.
2. The method according to claim 1, wherein the modified nano-modified polyurethane resin in step (1) is one or more of a polyurethane modified nano-modified polyurethane resin and a polyacrylate modified nano-modified polyurethane resin.
3. The method of claim 2, wherein the preparation method of the nano-modified polyurethane resin comprises the following steps:
according to the mass portion, 60-80 portions of polyester polyol with the number average molecular weight of 1000-4000 are heated to 110-130 ℃, vacuumized to-0.08 to-0.1 MPa, kept for 2-4h and then cooled to 45-60oC, introducing high-purity nitrogen to the standard atmospheric pressure, adding 30-40 parts of MDI (diphenylmethane diisocyanate) and 80-90 parts of MDIoC, reacting for 2-4h under the protection of nitrogen; after the reaction is finished, 3 to 8 parts of 1H,1H,12H, 12H-perfluoro-1, 12-dodecanediol and 0.1 to 0.5 part of stannous octoate are added, and the temperature is raised to 80 to 90oC, reaction 30-Cooling for 60min to 0-10oAnd C, adding 80-100 parts of solvent acetone, 5-10 parts of nano titanium oxide, 0.2-0.6 part of 2, 3-naphthalocyanine tin, 0.7-1.6 parts of KH-792 and 0.3-0.9 part of stearic acid monoglyceride, and performing high-speed shearing dispersion at 65-75 ℃ for 80-100min to obtain the nano modified polyurethane.
4. The method as claimed in claim 1, wherein the synergist in step (1) is prepared by:
according to the mass portion, 15-22 portions of glyoxal and 1.2-3.3 portions of 2- (thiophene-2-yl) phenol, 1.5-4.2 portions of (R) -1, 1-spiroindane-7, 7-diphenol, 100 portions of tetrahydrofuran are evenly stirred, the pH value of the solution is adjusted to be neutral by sodium hydroxide, the solution is continuously stirred for 20-90min at 60-70 ℃, then 1-4 portions of hexamethylenetetramine are added into a reaction kettle, and the mixture is stirred for 60-180min at room temperature; then slowly heating to 65-77 ℃, stirring for 15-30min, adjusting the pH value to 3-5, and carrying out heat preservation reaction for 150-200 min; after the reaction is finished, tetrahydrofuran is removed through reduced pressure distillation, and the synergist can be obtained.
5. The method according to claim 1, wherein the porous powder in step (1) is one or more of nano porous alumina, mesoporous silica, nano porous boron nitride and nano porous silicon carbide.
6. The method as claimed in claim 1, wherein the rust-proof pigment in step (1) is one or more of red lead powder, iron red powder, composite ferrotitanium powder, aluminum zinc tripolyphosphate powder and zinc caseinate.
7. The method of claim 1, wherein the dispersant is one or more of sodium oleate, oleyl oleate, pyridinium propanesulfonate, sodium polynaphthalenesulfonate, and sodium polyacrylate.
8. The method according to claim 1, wherein the defoaming agent is one or more of trialkyl melamine, cyanuric chloride melamine, dialkyl phosphate and fluorinated alkyl phosphate, palmitic acid and fatty glyceride.
9. The method of claim 1, wherein the anti-skinning agent is a combination of one or more of methyl ethyl ketoxime, turpentine, dipentene, diacetyl monoxime.
10. The method as claimed in claim 2, wherein the process parameters of the high efficiency multiple atomization arc spraying are 0.6MPa of atomization gas pressure and 2.5m of atomization gas flow3And/min, the spraying voltage is 33V, the spraying angle is 74 degrees, and the spraying distance is 200 mm.
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