CN119119853A - A high-strength corrosion-resistant coating for aircraft and preparation method thereof - Google Patents
A high-strength corrosion-resistant coating for aircraft and preparation method thereof Download PDFInfo
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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
- 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
- C09D5/08—Anti-corrosive paints
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Abstract
本发明涉及涂料技术领域，尤其涉及一种飞机用高强度耐腐蚀涂料及其制备方法。先将水性聚氨酯、钛白粉和改性氧化石墨烯加入水中，然后加入分散剂，搅拌均匀，得到预混料，然后向预混料中加入消泡剂、固化剂和光稳定剂，继续搅拌，即得。本发明飞机蒙皮涂料兼具良好的耐腐蚀性能和机械强度，能够适应恶劣的自然环境。The present invention relates to the technical field of coatings, and in particular to a high-strength corrosion-resistant coating for aircraft and a preparation method thereof. First, waterborne polyurethane, titanium dioxide and modified graphene oxide are added to water, and then a dispersant is added and stirred evenly to obtain a premix, and then a defoamer, a curing agent and a light stabilizer are added to the premix, and stirring is continued to obtain the premix. The aircraft skin coating of the present invention has both good corrosion resistance and mechanical strength, and can adapt to harsh natural environments.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a high-strength corrosion-resistant coating for an aircraft and a preparation method thereof.
Background
The aircraft skin paint is used for the decoration, camouflage and anti-corrosion protection of a base material of an aircraft, and is also an aviation paint product with the largest dosage. The natural environment of the aircraft is complex and various, and the aircraft is extremely easy to be corroded in severe natural environment, especially in high-humidity and high-salt-fog areas, and aluminum alloy, aluminum-lithium alloy, stainless steel and the like used for manufacturing the aircraft. Corrosion can initiate or grow fatigue cracks in metallic materials, thereby reducing the strength of the materials, which not only results in economic losses, but also presents serious safety problems, and thus corrosion has become a major factor in determining the structural integrity and life of aircraft. The coating is a main means of corrosion protection for skins and aircraft parts, and durable, durable high-performance coatings are a precondition for providing good corrosion protection.
The Chinese patent publication No. CN117343619 discloses a primary color paint for aircraft skin and a preparation method thereof, wherein the primary color paint for aircraft skin consists of a base material component A, a curing agent component B and a diluent component C, and the base material component A comprises the following components in parts by weight of polyester resin, toughening resin, titanium white, silicon dioxide, anti-sagging agent, wetting dispersant, drier, flatting agent, dimethylbenzene, butyl acetate and propylene glycol methyl ether acetate.
The Chinese patent publication No. CN104927591 discloses an aircraft skin finishing coating and a preparation method thereof, wherein the formula comprises the following components in parts by weight, namely polyester resin with high hydroxyl content, fluororesin, SCA modified polyester resin, organosilicon modified polyester resin, leveling aid, rheology control aid, catalyst, dimethylbenzene and butyl acetate. The prepared coating has good high-temperature resistance and low-temperature resistance.
Under severe natural environment, aluminum alloy, aluminum-lithium alloy, stainless steel and the like used for manufacturing an aircraft are extremely easy to corrode, and in the technical scheme, the aircraft skin coating is easy to corrode under severe weather conditions, so that the aircraft skin coating is caused to fall off, and the aircraft skin coating needs to be frequently repaired.
Disclosure of Invention
The invention provides the high-strength corrosion-resistant coating for the aircraft and the preparation method thereof in order to overcome the problems in the prior art. The aircraft skin paint has good corrosion resistance and mechanical strength, and can adapt to severe natural environments.
In order to achieve the above object, the present invention adopts the following technical scheme:
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight:
80-100 parts of aqueous polyurethane resin, 50-60 parts of titanium dioxide, 20-30 parts of modified graphene oxide, 1-3 parts of defoamer, 1-3 parts of curing agent, 1-3 parts of dispersing agent, 1-3 parts of light stabilizer and 90-120 parts of water.
In the technical scheme of the invention, the waterborne polyurethane is used as a bonding component of the aircraft skin coating, and the coating does not contain an organic solvent and is environment-friendly. Titanium dioxide is used as a filler of the paint. The lamellar structure of the graphene oxide can form a labyrinth effect stacked layer by layer in the coating, the labyrinth effect is filled in holes of the coating, moisture, oxygen and corrosive media in the environment are prevented from contacting a metal substrate, in addition, micropores and defects formed in the curing process of the coating can be blocked by the graphene oxide lamellar in the coating, the path of the corrosive media to the metal substrate is increased, and the corrosion rate is reduced.
Preferably, the defoaming agent is polyoxyethylene ether.
Preferably, the curing agent is an aqueous polyisocyanate.
Preferably, the dispersant is polyacrylic acid.
Preferably, the preparation method of the modified graphene oxide comprises the following steps:
1) Adding graphene into concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding potassium permanganate, heating to 70-75 ℃, adding hydrogen peroxide for oxidation reaction, filtering, washing and drying to obtain graphene oxide;
2) Adding graphene oxide into deionized water, carrying out ultrasonic vibration and uniform dispersion to obtain graphene oxide suspension, adding sodium hydroxide solution into the graphene oxide suspension, heating at 60-65 ℃ for 20-30min, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding alkali-treated graphene oxide into citric acid solution, heating for 1-2h at 70-80 ℃, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Adding a silane coupling agent KH-560 into a mixed solution of ethanol and water, heating and stirring to obtain a hydrolysate, adding the wrinkled graphene oxide into the hydrolysate, heating and stirring for reaction, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to obtain hyperbranched polyethyleneimine solution, adding coupling agent modified wrinkled graphene oxide into the hyperbranched polyethyleneimine solution, heating and stirring for reaction, filtering, washing and drying to obtain modified graphene oxide.
According to the technical scheme, the graphene oxide is added into the paint, so that the contact of moisture, oxygen and corrosive media in the environment with the metal substrate is blocked, and the paint has certain corrosion resistance. However, the graphene oxide has a planar structure, so that the barrier property of the graphene oxide to moisture and corrosive media is affected. In order to further improve the corrosion resistance of the coating, the graphene oxide is subjected to surface modification treatment, and the prepared graphene oxide is respectively subjected to alkali liquor and acid liquor treatment to obtain the graphene oxide with the wrinkled surface, wherein the wrinkled graphene oxide has larger surface area and surface roughness than common graphene oxide, and has better barrier property to moisture and corrosive media, so that the corrosion resistance of the coating is further improved.
As described above, the acid-base treatment is performed on the graphene oxide, so that the surface of the graphene oxide is wrinkled, and the barrier property of the graphene to moisture and corrosive media is improved. However, according to the test, the pleated graphene oxide is added into the coating, so that the corrosion resistance of the coating can be obviously improved, but the mechanical strength of the coating is obviously reduced, and the coating is cracked in the curing process. In order to solve the problems, the hyperbranched polyethyleneimine is grafted to the surface of the wrinkled graphene oxide through an epoxy silane coupling agent, the hyperbranched polyethyleneimine has a more branched structure and rich amino groups, molecular chains of the hyperbranched polyethyleneimine are inserted into polyurethane resin to play a role in reinforcing a similar skeleton, and residual hydroxyl groups of the polyurethane resin and amino groups on the hyperbranched polyethyleneimine form hydrogen bond acting force, so that the bonding acting force of the graphene and polyurethane is improved, the impact strength of a coating is improved, and the high-strength coating is obtained.
Preferably, the oxidation reaction time in the step 1) is 1 to 3 hours.
Preferably, the concentration of the sodium hydroxide solution in step 2) is 0.1 to 0.5wt%.
Preferably, the concentration of the citric acid solution in the step 3) is 1 to 3wt%.
Preferably, the reaction temperature in the step 5) is 80 ℃ and the reaction time is 2h;
the concentration of the hyperbranched polyethyleneimine solution is 0.8-2.3wt%.
In the technical scheme of the invention, experiments show that when the mass concentration of the hyperbranched polyethylene sub-solution is higher than 0.8%, sufficient hyperbranched polyethyleneimine can be grafted on the surface of the wrinkled graphene oxide, so that the coating has good mechanical strength. However, it was unexpectedly found during the experiment that when the mass concentration of the hyperbranched polyethylene sub-solution exceeds 2.3%, the curing time of the coating suddenly and greatly increases, probably because the surface of the wrinkled graphene oxide is grafted with excessive hyperbranched polyethyleneimine, a large amount of amino groups on the molecule of the hyperbranched polyethyleneimine have a hydrophilic effect, so that evaporation of water in the coating is hindered, and therefore, the mass concentration of the hyperbranched polyethylene sub-solution is controlled to be not more than 2.3%.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
Adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring to obtain the modified polyurethane foam.
The invention has the following beneficial effects:
1) The waterborne polyurethane is used as a bonding component of the aircraft skin coating, and the coating does not contain an organic solvent, so that the aircraft skin coating is environment-friendly;
2) Alkali liquor and acid liquor are respectively carried out on the prepared graphene oxide to obtain surface-wrinkled graphene oxide, wherein the wrinkled graphene oxide has larger surface area and surface roughness than common graphene oxide, and has better barrier property to moisture and corrosive media, so that the corrosion resistance of the coating is greatly improved;
3) The hyperbranched polyethyleneimine is grafted to the surface of the wrinkled graphene oxide through the epoxy silane coupling agent, the hyperbranched polyethyleneimine has more branched structures and rich amino groups, the molecular chains of the hyperbranched polyethyleneimine are inserted into polyurethane resin to play a similar skeleton reinforcing role, and in addition, residual hydroxyl groups of the polyurethane resin and amino groups on the hyperbranched polyethyleneimine form hydrogen bond acting force, so that the bonding acting force of graphene and polyurethane is improved, the strength of a coating is improved, and the high-strength coating is obtained.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
The raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art unless otherwise specified, and the methods used in the examples of the present invention are all known to those skilled in the art.
In a specific embodiment, the light stabilizer used is Eversorb ℃ of the AQ1 light stabilizer produced permanently. The molecular weight of the hyperbranched polyethyleneimine is 100000Da.
Example 1
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight (see table 1):
Table 1 first weight part table of high strength corrosion resistant coating for aircraft
The preparation method of the modified graphene oxide comprises the following steps:
1) Adding 3g of graphene into 200mL of concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding 5g of potassium permanganate, heating to 73 ℃, adding 100mL of hydrogen peroxide with mass concentration of 20% for oxidation reaction for 2h, filtering, washing and drying to obtain graphene oxide;
2) Adding 2g of graphene oxide into 100mL of deionized water, carrying out ultrasonic oscillation and uniform dispersion to obtain graphene oxide suspension, adding 100mL of sodium hydroxide solution with mass concentration of 0.4wt% into the graphene oxide suspension, heating at 63 ℃ for 25min, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding 2g of alkali-treated graphene oxide into 300mL of citric acid aqueous solution with mass concentration of 2.5wt%, heating at 75 ℃ for 1.5h, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Mixing 100mL of ethanol and 10mL of water uniformly, adding 1g of silane coupling agent KH-560 into the mixed solution of ethanol and water, heating to 40 ℃, stirring for 30min to obtain hydrolysate, adding 2g of wrinkled graphene oxide into the hydrolysate, heating to 50 ℃, stirring for reacting for 2h, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to prepare hyperbranched polyethyleneimine solution with the mass concentration of 2.0wt%, adding 2g of coupling agent modified pleated graphene oxide into 500mL of hyperbranched polyethyleneimine solution, heating to 80 ℃, stirring and reacting for 2 hours, filtering, washing and drying to obtain modified graphene oxide.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring for 30min at 800r/min to obtain the modified polyurethane foam.
Example 2
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight (see table 2):
table 2 second weight part table of high strength corrosion resistant coating for aircraft
The preparation method of the modified graphene oxide comprises the following steps:
1) Adding 3g of graphene into 200mL of concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding 5g of potassium permanganate, heating to 73 ℃, adding 100mL of hydrogen peroxide with mass concentration of 20% for oxidation reaction for 2h, filtering, washing and drying to obtain graphene oxide;
2) Adding 2g of graphene oxide into 100mL of deionized water, carrying out ultrasonic oscillation and uniform dispersion to obtain graphene oxide suspension, adding 100mL of sodium hydroxide solution with mass concentration of 0.3wt% into the graphene oxide suspension, heating at 63 ℃ for 25min, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding 2g of alkali-treated graphene oxide into 300mL of citric acid aqueous solution with mass concentration of 1.5wt%, heating at 75 ℃ for 1.5h, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Mixing 100mL of ethanol and 10mL of water uniformly, adding 1g of silane coupling agent KH-560 into the mixed solution of ethanol and water, heating to 40 ℃, stirring for 30min to obtain hydrolysate, adding 2g of wrinkled graphene oxide into the hydrolysate, heating to 50 ℃, stirring for reacting for 2h, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to prepare hyperbranched polyethyleneimine solution with the mass concentration of 1.0wt%, adding 2g of coupling agent modified pleated graphene oxide into 500mL of hyperbranched polyethyleneimine solution, heating to 80 ℃, stirring and reacting for 2 hours, filtering, washing and drying to obtain modified graphene oxide.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring for 30min at 800r/min to obtain the modified polyurethane foam.
Example 3
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight (see table 3):
Table 3 third weight part table of high strength corrosion resistant coating for aircraft
The preparation method of the modified graphene oxide comprises the following steps:
1) Adding 3g of graphene into 200mL of concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding 5g of potassium permanganate, heating to 73 ℃, adding 100mL of hydrogen peroxide with mass concentration of 20% for oxidation reaction for 2h, filtering, washing and drying to obtain graphene oxide;
2) Adding 2g of graphene oxide into 100mL of deionized water, carrying out ultrasonic oscillation and uniform dispersion to obtain graphene oxide suspension, adding 100mL of sodium hydroxide solution with mass concentration of 0.3wt% into the graphene oxide suspension, heating at 63 ℃ for 25min, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding 2g of alkali-treated graphene oxide into 300mL of citric acid aqueous solution with mass concentration of 2wt%, heating at 75 ℃ for 1.5h, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Mixing 100mL of ethanol and 10mL of water uniformly, adding 1g of silane coupling agent KH-560 into the mixed solution of ethanol and water, heating to 40 ℃, stirring for 30min to obtain hydrolysate, adding 2g of wrinkled graphene oxide into the hydrolysate, heating to 50 ℃, stirring for reacting for 2h, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to prepare hyperbranched polyethyleneimine solution with the mass concentration of 1.5wt%, adding 2g of coupling agent modified pleated graphene oxide into 500mL of hyperbranched polyethyleneimine solution, heating to 80 ℃, stirring and reacting for 2 hours, filtering, washing and drying to obtain modified graphene oxide.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring for 30min at 800r/min to obtain the modified polyurethane foam.
Example 4
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight (see table 4):
Table 4 fourth weight part table of high strength corrosion resistant coating for aircraft
The preparation method of the modified graphene oxide comprises the following steps:
1) Adding 3g of graphene into 200mL of concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding 5g of potassium permanganate, heating to 75 ℃, adding 100mL of hydrogen peroxide with mass concentration of 20% for oxidation reaction for 3h, filtering, washing and drying to obtain graphene oxide;
2) Adding 2g of graphene oxide into 100mL of deionized water, carrying out ultrasonic oscillation and uniform dispersion to obtain graphene oxide suspension, adding 100mL of sodium hydroxide solution with mass concentration of 0.5wt% into the graphene oxide suspension, heating for 30min at 65 ℃, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding 2g of alkali-treated graphene oxide into 300mL of citric acid aqueous solution with mass concentration of 3wt%, heating for 2 hours at 80 ℃, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Mixing 100mL of ethanol and 10mL of water uniformly, adding 1g of silane coupling agent KH-560 into the mixed solution of ethanol and water, heating to 40 ℃, stirring for 30min to obtain hydrolysate, adding 2g of wrinkled graphene oxide into the hydrolysate, heating to 50 ℃, stirring for reacting for 2h, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to prepare hyperbranched polyethyleneimine solution with the mass concentration of 2.3wt%, adding 2g of coupling agent modified pleated graphene oxide into 500mL of hyperbranched polyethyleneimine solution, heating to 80 ℃, stirring and reacting for 2 hours, filtering, washing and drying to obtain modified graphene oxide.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring for 30min at 800r/min to obtain the modified polyurethane foam.
Example 5
The high-strength corrosion-resistant coating for the aircraft comprises the following components in parts by weight (see table 5):
Table 5 fifth weight part table of high strength corrosion resistant coating for aircraft
The preparation method of the modified graphene oxide comprises the following steps:
1) Adding 3g of graphene into 200mL of concentrated sulfuric acid under ice bath condition, stirring uniformly, then adding 5g of potassium permanganate, heating to 70 ℃, adding 100mL of hydrogen peroxide with mass concentration of 20% for oxidation reaction for 1h, filtering, washing and drying to obtain graphene oxide;
2) Adding 2g of graphene oxide into 100mL of deionized water, carrying out ultrasonic oscillation and uniform dispersion to obtain graphene oxide suspension, adding 100mL of sodium hydroxide solution with mass concentration of 0.1wt% into the graphene oxide suspension, heating at 60 ℃ for 20min, and carrying out centrifugal separation, washing and drying to obtain alkali-treated graphene oxide;
3) Adding 2g of alkali-treated graphene oxide into 300mL of citric acid aqueous solution with mass concentration of 1wt%, heating for 1h at 70 ℃, and performing centrifugal separation, washing and drying to obtain wrinkled graphene oxide;
4) Mixing 100mL of ethanol and 10mL of water uniformly, adding 1g of silane coupling agent KH-560 into the mixed solution of ethanol and water, heating to 40 ℃, stirring for 30min to obtain hydrolysate, adding 2g of wrinkled graphene oxide into the hydrolysate, heating to 50 ℃, stirring for reacting for 2h, and performing centrifugal separation, washing and drying to obtain coupling agent modified wrinkled graphene oxide;
5) Adding hyperbranched polyethyleneimine into deionized water, stirring and dissolving to prepare hyperbranched polyethyleneimine solution with the mass concentration of 0.8wt%, adding 2g of coupling agent modified pleated graphene oxide into 500mL of hyperbranched polyethyleneimine solution, heating to 80 ℃, stirring and reacting for 2 hours, filtering, washing and drying to obtain modified graphene oxide.
A preparation method of the high-strength corrosion-resistant coating for the aircraft comprises the following steps:
adding waterborne polyurethane, titanium dioxide and modified graphene oxide into water, then adding a dispersing agent, and uniformly stirring to obtain a premix;
adding the defoaming agent, the curing agent and the light stabilizer into the premix, and continuously stirring for 30min at 800r/min to obtain the modified polyurethane foam.
Comparative example 1:
comparative example 1 differs from example 1 in that:
the preparation process of the modified graphene oxide only comprises the step 1), and other preparation steps are omitted.
The remaining operation procedure was the same as in example 1.
Comparative example 2:
comparative example 2 differs from example 1 in that:
step 4) and step 5) are omitted in the preparation process of the modified graphene oxide).
The remaining operation procedure was the same as in example 1.
Comparative example 3:
Comparative example 3 differs from example 5 in that:
In the step 5) of the preparation process of the modified graphene oxide, the concentration of the prepared hyperbranched polyethyleneimine solution is 0.7 weight percent.
The remaining procedure was the same as in example 5.
Comparative example 4:
comparative example 4 differs from example 4 in that:
In the step 5) of the preparation process of the modified graphene oxide, the concentration of the prepared hyperbranched polyethyleneimine solution is 2.4 weight percent.
The remaining procedure was the same as in example 4.
Comparative example 5:
comparative example 5 differs from example 4 in that:
in the step 5) of the preparation process of the modified graphene oxide, the concentration of the prepared hyperbranched polyethyleneimine solution is 2.5 weight percent.
The remaining procedure was the same as in example 4.
Performance test:
film preparation is carried out according to the specification of GB/T1727-1992 general preparation method of paint film, the surface drying and the real drying time of the film are tested under the conditions of 50 ℃ and 50% relative humidity, and after curing for 7d under the standard temperature and humidity, whether the surface of the film is cracked or not is observed, and each performance of the film is detected.
1, Pencil hardness test, namely, testing according to GB/T6739-1996 'film hardness pencil test method', and selecting a Chinese pencil with the model of 2B-6H to test on a pencil hardness test bed. Each sample plate is tested three times, and the lowest hardness is taken as a final test result.
Impact resistance test according to GB/T1732-1993 "film impact resistance test", impact tests were carried out by selecting different heights using an impact tester. 3 points were selected for impact testing for each panel, with one point passing no more than one. And selecting a proper impact height for further testing, and finally obtaining a result.
And 3, adhesive force test, namely uniformly coating the coating on a steel plate by adopting a 10 mu m wire rod, then putting the steel plate into a 50 ℃ oven to dry the coating, dividing the coating, peeling the coating by using a transparent adhesive tape, judging the adhesive force grade of the coating according to the damage degree, and grading the coating into 0-5 grids according to the damage degree, wherein the grade of 0-5 indicates that the adhesive force is gradually deteriorated.
And 4, testing corrosion resistance, namely adding 5g of citric acid into 1000mL of deionized water, stirring and dissolving to obtain an acidic solution, soaking the prepared coating in the acidic solution for 60 days, taking out, drying, and observing whether corrosion occurs on the surface of the coating.
The results of the above test data are shown in Table 6:
Table 6 test data results table
The corrosion resistance of the paint prepared in the examples 1-5 is superior to that of the paint prepared in the comparative example 1, because the graphene oxide in the examples 1-5 is treated by alkali liquor and acid liquor respectively to obtain the graphene oxide with wrinkled surfaces, the wrinkled graphene oxide has larger surface area and surface roughness than the common graphene oxide, and has better barrier property to moisture and corrosive media, so that the corrosion resistance of the paint is further improved.
The test data of the examples 1-5 and the comparative example 2 can be compared to obtain that the impact resistance of the coating prepared in the examples 1-5 is superior to that of the coating prepared in the comparative example 2, because the hyperbranched polyethyleneimine is grafted to the surface of the wrinkled graphene oxide through the epoxy silane coupling agent in the examples 1-5, the hyperbranched polyethyleneimine has more branched structures and rich amino groups, the molecular chains of the hyperbranched polyethyleneimine are interpenetrated in polyurethane resin to play a similar role in skeleton reinforcement, and in addition, the residual hydroxyl groups of the polyurethane resin and the amino groups on the hyperbranched polyethyleneimine form hydrogen bond acting force, so that the bonding acting force of graphene and polyurethane is improved, and the impact resistance of the coating is improved.
As can be seen from the comparison of the test data of examples 1-5 and comparative example 3, the impact strength of the coatings of examples 1-5 is higher than that of comparative example 3, which is that the amount of hyperbranched polyethyleneimine grafted on the surface of the wrinkled graphene oxide in comparative example 3 is insufficient, and the skeleton enhancement effect formed by the hyperbranched polyethyleneimine is weaker, so that the impact strength of the coating is reduced.
From comparison of the test data of examples 1-5 with comparative examples 4-5, it can be seen that the example 1-5 coatings were significantly shorter in curing time than comparative examples 4 and 5, probably because the surface grafting of the wrinkled graphene oxide with an excessive amount of hyperbranched polyethyleneimine, the large number of amino groups on the molecule of which had a hydrophilic effect, thereby hindering evaporation of water in the coatings.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
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|---|---|---|---|---|
| CN120590600A (en) * | 2025-06-23 | 2025-09-05 | 三晃树脂（佛山）有限公司 | A low-temperature resistant water-based polyurethane |
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| CN119119853B (en) | 2025-05-09 |
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