CN111701831A - Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel - Google Patents

Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel Download PDF

Info

Publication number
CN111701831A
CN111701831A CN202010629985.XA CN202010629985A CN111701831A CN 111701831 A CN111701831 A CN 111701831A CN 202010629985 A CN202010629985 A CN 202010629985A CN 111701831 A CN111701831 A CN 111701831A
Authority
CN
China
Prior art keywords
carbon steel
hydrophobic silica
minutes
hydrophobic
epoxy resin
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010629985.XA
Other languages
Chinese (zh)
Inventor
徐杨书函
高大明
董强
刘安求
王晓晨
王淑芬
刘峤
何吉喆
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hefei University
Original Assignee
Hefei University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hefei University filed Critical Hefei University
Priority to CN202010629985.XA priority Critical patent/CN111701831A/en
Publication of CN111701831A publication Critical patent/CN111701831A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14Processes, 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
    • B05D7/16Processes, 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50Multilayers
    • B05D7/51One specific pretreatment, e.g. phosphatation, chromatation, in combination with one specific coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2504/00Epoxy polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses a preparation method of a hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel, which is characterized by comprising the following operation steps of: (1) mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 5-10 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nanoparticles to the absolute ethyl alcohol is controlled to be 1: 50-1: 4; (2) adding a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether into the mixed solution A, and then mixing and stirring for 10-15 minutes to obtain mixed solution B; the pollution in the coating preparation process is small, the coating preparation process conditions are mild, the temperature required by the coating during heat treatment is not high, the hydrophobic silicon dioxide is added into the composite coating, the hydrophobic silicon dioxide can slow down the diffusion of a corrosion medium in the anticorrosive thin film, and the anticorrosive performance of the anticorrosive thin film is further improved.

Description

Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel
Technical Field
The invention relates to the technical field of anticorrosive coatings, in particular to a preparation method of a hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel.
Background
Corrosion and fouling problems are widespread in many areas including the transport of fluids in pipelines, heat exchange processes in heat exchangers, and marine transport. Corrosion and fouling will lead to blockage and damage of the pipelines, a decrease in the heat exchange efficiency of the heat exchangers and an increase in the resistance to sailing in the sea and damage to the ship hull. The data show that the loss caused by the corrosion of metal materials in China accounts for 5 percent of GDP every year, and the economic loss caused by China is about 5000 billion yuan every year. In addition, the annual metal material corrosion results in about 10% -20% metal loss, and if calculated according to one hundred million tons of steel produced per year, 1000 million tons of steel are corroded per year, and the number is equivalent to the annual steel production of a large steel enterprise, so that the severity of resource consumption caused by metal corrosion can be seen. Therefore, the development of a coating layer with stronger corrosion resistance, anti-scaling property and less environmental pollution brings benefits and convenience to many fields.
The sol-gel technique, which is often used to prepare ceramic coatings, has attracted much attention in coating preparation, mainly because of the low sintering temperature and easy processability of this method. These ceramic coatings include zirconia coatings, titania coatings, zinc oxide coatings and silica coatings, which have been reported as corrosion resistant coatings, but defects in the coating surface such as cracking and excessively thin film thickness affect the corrosion resistance of these coatings. An yttria-stabilized zirconia coating has been reported for use in the preparation of corrosion-resistant films on commercial carbon steels. According to the scanning electron microscope, the surface of the prepared film had severe cracks. This yttria-stabilized zirconia coating sintered at 673K lost its corrosion resistance after only 3 days of immersion in a 3.5 wt.% sodium chloride solution. Recently, many silicone organic coatings have been prepared for corrosion protection by hydrolytic polycondensation of silanes due to their non-toxicity, chemical stability and thermal stability. Although these organopolysiloxane coatings are also prepared by sol-gel methods, these coatings exhibit better corrosion resistance than ceramic coatings because of the introduction of organic functional groups. For organopolysiloxane coatings, the coating has a much better micro-morphology and corrosion resistance than ceramic coatings. An organopolysiloxane composite coating by synergistically mixing tetraethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane and methyl methacrylate has been reported as a corrosion protection coating. Such a coating without the addition of methyl methacrylate exhibits a very good microstructure. In terms of corrosion protection, the low band impedance value in the electrochemical impedance spectrum of the coated coupon after immersion in a 3.5 wt.% sodium chloride solution for 96 hours was still 10 times the impedance value of the uncoated coupon. In addition, thick silicone coatings with high hardness can also be produced by the sol-gel process of the organoalkylsilanes at room temperature. Therefore organopolysiloxane coatings would be more available for use as corrosion protection coatings.
In addition to the silicone coatings that have attracted much attention in recent years, epoxy coatings are also commonly used as corrosion protection coatings. Epoxy resins have attracted much attention as an organic polymer coating due to their outstanding adhesion, high corrosion resistance and environmental friendliness. In general, the epoxy may act as a physical barrier to the intrusion of harmful substances. But the original epoxy resin does not provide long-term corrosion protection due to the presence of pores and defects in the coating after the curing process that allow oxygen, water and corrosive particles (e.g., chloride and hydrogen ions) to penetrate into the coating. Recently, inorganic nanofillers such as silica, zirconia, zinc oxide and nanoclay have been introduced into epoxy matrices to form epoxy nanocomposites and have been used to modify the physical barrier effect of epoxy resins, which is used to further advance the anti-corrosion properties of epoxy resins. It has been reported that nanoparticles can fill voids, microcracks, and defects in epoxy coatings, which can lead to better corrosion protection characteristics. For example, Sari et al prepared polyesteramide hyperbranched polymer-modified nanoclay particles that act as a nano-filler to enhance the dispersion characteristics of nanoclay in an epoxy resin matrix, and epoxy resins filled with the modified nanoclay particles achieved improved corrosion resistance characteristics. Pure nanoclay is hydrophilic, which results in agglomeration of nanoparticles and poor intercalation. However, the nanoclay modified with the polyester amide hyperbranched polymer exhibits uniform particle dispersibility in the epoxy resin coating, which may effectively extend the diffusion path of corrosive electrolytes such as chloride ions, oxygen and water. The search for new advanced modification methods and new nanofillers for epoxy nanocomposite coatings would be a future task for researchers in the field of corrosion protection.
More recently, hydrophobic surfaces have also been reported to have corrosion protection properties. These hydrophobic surfaces can be obtained by one-step platinum displacement, self-assembly of octadecyltrimethoxysiloxane, electrodeposition of textured polythiophenes, spraying of reaction products of metal salts with alkyl thiols, chemical modification of stearic or myristic acid, dip coating of polypropylene and self-assembly of fluorinated alkyl silanes, etc. The corrosion resistance of a hydrophobic surface can be attributed to the air layer trapped at the valleys of the rough surface. This trapped air will reduce the actual contact area between the rough surface and the water and prevent corrosive media from reaching the surface. Thus, metals with hydrophobic surfaces generally exhibit better corrosion resistance. In addition, these hydrophobic surfaces may also exhibit anti-fouling properties, including dust, graphite powder, alumina powder, calcium carbonate scale, and calcium sulfate scale. The air layer of the hydrophobic surface may also block the transmission of dirt particles.
Since the hydrophobicity of the hydrophobic coating can enhance the corrosion resistance of the coating in an aqueous medium, we can naturally think that the corrosion resistance of the coating will be further enhanced if the hydrophobic character is imparted to a conventional corrosion-resistant coating.
Therefore, it is necessary to invent a preparation method of the hydrophobic silica nanoparticle modified epoxy resin anticorrosive thin film to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrophobic silica nanoparticle modified epoxy resin anticorrosive film, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel is characterized by comprising the following operation steps:
(1) mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 5-10 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nanoparticles to the absolute ethyl alcohol is controlled to be 1: 50-1: 4;
(2) and adding a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether into the mixed liquid A, and mixing and stirring for 10-15 minutes to obtain a mixed liquid B. Wherein the total mass of the added diethylenetriamine and the trimethylolpropane triglycidyl ether is the same as that of the absolute ethyl alcohol used in the step (1), and the mass ratio of the diethylenetriamine to the trimethylolpropane triglycidyl ether is controlled to be 1: 8-1: 6;
(3) and (3) placing the mixed solution B in an ultrasonic cleaning machine for ultrasonic treatment for 3-5 minutes so as to better disperse the hydrophobic silicon dioxide nano particles in the mixed solution B. Wherein the ultrasonic frequency during ultrasonic treatment is 40 kHz;
(4) the carbon steel to be coated with the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film is firstly subjected to phosphating treatment, so that a layer of uniform and compact phosphating film is formed on the surface of the carbon steel. The main purpose of forming the phosphating film is to allow the anticorrosive film to be better coated on the surface of the substrate;
(5) immersing phosphatized carbon steel into the mixed liquid B at a speed of 3000-5000 [ mu ] m/s in a dip-coating mode, staying for 0.5-2 minutes after immersion, and then lifting out the carbon steel from the mixed liquid B at a speed of 1000-3000 [ mu ] m/s;
(6) and (3) placing the pulled sample wafer in an oven for heat treatment at the temperature of 80-120 ℃ for 90-120 minutes, and taking out the sample wafer to obtain the carbon steel sample wafer coated with the hydrophobic silicon dioxide nano particle modified epoxy resin anticorrosive film.
Preferably, the mixed solution B may be applied to the surface of the sample substrate by brushing, spraying, spin coating, or the like.
The invention has the technical effects and advantages that:
the coating preparation process has the advantages of small pollution, relatively simple coating preparation process, relatively mild coating preparation process conditions, low temperature required during coating heat treatment, and hydrophobic silica added in the composite coating, and can slow down the diffusion of corrosive media in the anticorrosive film, thereby further improving the anticorrosive performance of the anticorrosive film.
Drawings
Fig. 1 is an electrochemical impedance spectrum of the coating prepared in example 1 of the present invention immersed in a 3.5 wt.% sodium chloride solution for various periods of time, and it can be seen from the graph that the impedance at the low frequency band (f = 0.01 Hz) of the impedance spectrum is about 5.3 × 105 Ω · cm2 immediately after immersion of the coupon in the sodium chloride solution, and the impedance at the low frequency band (f = 0.01 Hz) of the impedance spectrum decreases to about 4700 Ω · cm2 after immersion for 1367 hours (about 57 days) in the sodium chloride solution.
Fig. 2 is an electrochemical impedance spectrum of the coating prepared in example 2 of the present invention immersed in a 3.5 wt.% sodium chloride solution for various periods of time, and it can be seen that the impedance of the sample wafer at the low frequency band (f = 0.01 Hz) of the impedance spectrum is about 8.7 × 104 Ω · cm2 immediately after immersion in the sodium chloride solution, and the impedance of the sample wafer at the low frequency band (f = 0.01 Hz) of the impedance spectrum decreases to about 300 Ω · cm2 after immersion in the sodium chloride solution for 143 hours (about 6 days). It can be seen that the corrosion resistance of the coating prepared in example 2 is significantly weaker than that of example 1.
Fig. 3 is an electrochemical impedance spectrum of the coating prepared in example 3 of the present invention immersed in a 3.5 wt.% sodium chloride solution for various periods of time, and it can be seen from the graph that the impedance at the low frequency band (f = 0.01 Hz) of the impedance spectrum is about 3.9 × 104 Ω · cm2 immediately after immersion of the coupon in the sodium chloride solution, and the impedance at the low frequency band (f = 0.01 Hz) of the impedance spectrum decreases to about 96 Ω · cm2 after immersion for 143 hours (about 6 days) in the sodium chloride solution. It can be seen that the corrosion resistance of the coating prepared in example 3 is much weaker than that of example 2 and much weaker than that of example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 10 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nano particles to the absolute ethyl alcohol is controlled to be 1: 4.5.
(2) To the mixture liquid a, a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether were added, followed by mixing and stirring for 15 minutes to obtain a mixture liquid B. Wherein the total mass of diethylenetriamine and trimethylolpropane triglycidyl ether added is the same as the total mass of absolute ethanol used in the step (1), and the mass ratio of diethylenetriamine and trimethylolpropane triglycidyl ether is controlled to 1: 7.
(3) And (3) placing the mixed solution B in an ultrasonic cleaning machine for ultrasonic treatment for 5 minutes to better disperse the hydrophobic silica nano particles in the mixed solution B. Wherein the ultrasonic frequency in the ultrasonic treatment is 40 kHz.
(4) The carbon steel to be coated with the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film is firstly subjected to phosphating treatment, so that a layer of uniform and compact phosphating film is formed on the surface of the carbon steel. The main purpose of forming the phosphating film is to allow the anticorrosive film to be better coated on the surface of the substrate.
(5) And immersing the phosphatized carbon steel into the mixed liquid B at a speed of 3000 mu m/s in a dip-coating mode, staying for 0.5 min after immersion, and then lifting and pulling out the carbon steel from the mixed liquid B at a speed of 2000 mu m/s.
(6) And (3) placing the pulled sample wafer in an oven for heat treatment at 80 ℃ for 90 minutes, and taking out the sample wafer to obtain the carbon steel sample wafer coated with the hydrophobic silicon dioxide nano particle modified epoxy resin anticorrosive film.
The prepared coating is gray black, uniform in texture and free of cracking, the surface of the coating is rough, no reflection exists under the irradiation of light, the adhesion with a substrate is good, and the thickness of the prepared film is about 12 microns.
Example 2
(1) Mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 5 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nano particles to the absolute ethyl alcohol is controlled to be 1: 10.
(2) To the mixture liquid a, a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether were added, followed by mixing and stirring for 10 minutes to obtain a mixture liquid B. Wherein the total mass of diethylenetriamine and trimethylolpropane triglycidyl ether added is the same as the total mass of absolute ethanol used in the step (1), and the mass ratio of diethylenetriamine and trimethylolpropane triglycidyl ether is controlled to 1: 6.
(3) And (3) placing the mixed solution B in an ultrasonic cleaning machine for ultrasonic treatment for 3 minutes to better disperse the hydrophobic silica nano particles in the mixed solution B. Wherein the ultrasonic frequency in the ultrasonic treatment is 40 kHz.
(4) The carbon steel to be coated with the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film is firstly subjected to phosphating treatment, so that a layer of uniform and compact phosphating film is formed on the surface of the carbon steel. The main purpose of forming the phosphating film is to allow the anticorrosive film to be better coated on the surface of the substrate.
(5) And immersing the phosphatized carbon steel into the mixed liquid B at a speed of 5000 [ mu ] m/s in a dip-coating mode, staying for 2 minutes after immersion, and then lifting and pulling out the carbon steel from the mixed liquid B at a speed of 3000 [ mu ] m/s.
(6) And (3) placing the pulled sample wafer in an oven for heat treatment at 120 ℃ for 120 minutes, and taking out the sample wafer to obtain the carbon steel sample wafer coated with the hydrophobic silicon dioxide nano particle modified epoxy resin anticorrosive film.
The prepared coating is gray black, uniform in texture and free of cracking, the roughness of the coating is moderate, light is reflected under the irradiation of light, the adhesion with a substrate is good, and the thickness of the prepared film is about 12 microns.
Example 3
(1) Mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 8 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nano particles to the absolute ethyl alcohol is controlled to be 1: 49.5.
(2) To the mixture liquid a, a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether were added, followed by mixing and stirring for 12 minutes to obtain a mixture liquid B. Wherein the total mass of diethylenetriamine and trimethylolpropane triglycidyl ether added is the same as the total mass of absolute ethanol used in the step (1), and the mass ratio of diethylenetriamine and trimethylolpropane triglycidyl ether is controlled to 1: 8.
(3) And (3) placing the mixed solution B in an ultrasonic cleaning machine for ultrasonic treatment for 4 minutes to better disperse the hydrophobic silica nano particles in the mixed solution B. Wherein the ultrasonic frequency in the ultrasonic treatment is 40 kHz.
(4) The carbon steel to be coated with the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film is firstly subjected to phosphating treatment, so that a layer of uniform and compact phosphating film is formed on the surface of the carbon steel. The main purpose of forming the phosphating film is to allow the anticorrosive film to be better coated on the surface of the substrate.
(5) And immersing the phosphatized carbon steel into the mixed liquid B at the speed of 4000μm/s in a dip-coating mode, staying for 1 minute after immersion, and then lifting and pulling out the carbon steel from the mixed liquid B at the speed of 1000μm/s.
(6) And (3) placing the pulled sample wafer in an oven for 100 minutes of heat treatment at 100 ℃, and taking out the sample wafer to obtain the carbon steel sample wafer coated with the hydrophobic silicon dioxide nano particle modified epoxy resin anticorrosive film.
The prepared coating is gray black, uniform in texture and free of cracking, the coating is smooth, has light reflection under the irradiation of light, and has good adhesion with a substrate, and the thickness of the prepared film is about 10 microns.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (2)

1. A preparation method of a hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel is characterized by comprising the following operation steps:
(1) mixing and stirring a certain amount of hydrophobic silicon dioxide nano particle powder and absolute ethyl alcohol for 5-10 minutes to obtain a mixed solution A. Wherein the particle size of the hydrophobic silica nanoparticles is about 300 nanometers. The mass ratio of the hydrophobic silica nanoparticles to the absolute ethyl alcohol is controlled to be 1: 50-1: 4;
(2) and adding a certain amount of diethylenetriamine and trimethylolpropane triglycidyl ether into the mixed liquid A, and mixing and stirring for 10-15 minutes to obtain a mixed liquid B. Wherein the total mass of the added diethylenetriamine and the trimethylolpropane triglycidyl ether is the same as that of the absolute ethyl alcohol used in the step (1), and the mass ratio of the diethylenetriamine to the trimethylolpropane triglycidyl ether is controlled to be 1: 8-1: 6;
(3) and (3) placing the mixed solution B in an ultrasonic cleaning machine for ultrasonic treatment for 3-5 minutes so as to better disperse the hydrophobic silicon dioxide nano particles in the mixed solution B. Wherein the ultrasonic frequency during ultrasonic treatment is 40 kHz;
(4) the carbon steel to be coated with the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film is firstly subjected to phosphating treatment, so that a layer of uniform and compact phosphating film is formed on the surface of the carbon steel. The main purpose of forming the phosphating film is to allow the anticorrosive film to be better coated on the surface of the substrate;
(5) immersing phosphatized carbon steel into the mixed liquid B at a speed of 3000-5000 [ mu ] m/s in a dip-coating mode, staying for 0.5-2 minutes after immersion, and then lifting out the carbon steel from the mixed liquid B at a speed of 1000-3000 [ mu ] m/s;
(6) and (3) placing the pulled sample wafer in an oven for heat treatment at the temperature of 80-120 ℃ for 90-120 minutes, and taking out the sample wafer to obtain the carbon steel sample wafer coated with the hydrophobic silicon dioxide nano particle modified epoxy resin anticorrosive film.
2. The preparation method of the hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on the carbon steel according to claim 1, characterized in that: the mixed solution B can also be coated on the surface of the sample substrate by brushing, spraying, spin coating and the like.
CN202010629985.XA 2020-07-03 2020-07-03 Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel Pending CN111701831A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010629985.XA CN111701831A (en) 2020-07-03 2020-07-03 Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010629985.XA CN111701831A (en) 2020-07-03 2020-07-03 Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel

Publications (1)

Publication Number Publication Date
CN111701831A true CN111701831A (en) 2020-09-25

Family

ID=72546122

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010629985.XA Pending CN111701831A (en) 2020-07-03 2020-07-03 Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel

Country Status (1)

Country Link
CN (1) CN111701831A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113583543A (en) * 2021-09-02 2021-11-02 苏州科技大学 Preparation method and application of hydrophobic composite anti-corrosion coating

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1597775A (en) * 2004-08-26 2005-03-23 长江水利委员会长江科学院 Preparation technology for composite of epoxy resin nano silicon dioxide
CN1766019A (en) * 2005-09-22 2006-05-03 长江水利委员会长江科学院 Nano composite aqueous epoxide resin coating material and preparation method
CN104797622A (en) * 2012-11-16 2015-07-22 陶氏环球技术有限公司 Epoxy resin compositions
CN105026154A (en) * 2013-03-06 2015-11-04 E.I.内穆尔杜邦公司 A printing form and a process for preparing a printing form using two-step cure
CN105837797A (en) * 2016-04-08 2016-08-10 苏州圣杰特种树脂有限公司 A water-based epoxy resin curing agent
CN109306150A (en) * 2018-10-17 2019-02-05 安徽菲扬新材料有限公司 A kind of preparation method of room temperature curing epoxy composite material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1597775A (en) * 2004-08-26 2005-03-23 长江水利委员会长江科学院 Preparation technology for composite of epoxy resin nano silicon dioxide
CN1766019A (en) * 2005-09-22 2006-05-03 长江水利委员会长江科学院 Nano composite aqueous epoxide resin coating material and preparation method
CN104797622A (en) * 2012-11-16 2015-07-22 陶氏环球技术有限公司 Epoxy resin compositions
CN105026154A (en) * 2013-03-06 2015-11-04 E.I.内穆尔杜邦公司 A printing form and a process for preparing a printing form using two-step cure
CN105837797A (en) * 2016-04-08 2016-08-10 苏州圣杰特种树脂有限公司 A water-based epoxy resin curing agent
CN109306150A (en) * 2018-10-17 2019-02-05 安徽菲扬新材料有限公司 A kind of preparation method of room temperature curing epoxy composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵俊伟等: "二氧化硅/环氧树脂复合涂层的制备及其疏水性能", 《化学研究》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113583543A (en) * 2021-09-02 2021-11-02 苏州科技大学 Preparation method and application of hydrophobic composite anti-corrosion coating

Similar Documents

Publication Publication Date Title
CN109852972B (en) Anticorrosive carbon nanotube/silane composite super-hydrophobic coating and preparation method thereof
Zhao et al. Environmentally-friendly superhydrophobic surface based on Al2O3@ KH560@ SiO2 electrokinetic nanoparticle for long-term anti-corrosion in sea water
Yu et al. Corrosion resistance of three-layer superhydrophobic composite coating on carbon steel in seawater
Liu et al. Corrosion protection of silane coatings modified by carbon nanotubes on stainless steel
Durán et al. Protection and surface modification of metals with sol–gel coatings
Jianguo et al. Enhancement of the erosion–corrosion resistance of Dacromet with hybrid SiO2 sol–gel
Zhang et al. Superhydrophobic surface on Al alloy with robust durability and excellent self-healing performance
Zhan-Fang et al. Super-hydrophobic coating used in corrosion protection of metal material: review, discussion and prospects
CN111701831A (en) Preparation method of hydrophobic silica nanoparticle modified epoxy resin anticorrosive film coated on carbon steel
Fan et al. Development of superhydrophobic and corrosion resistant coatings on carbon steel by hydrothermal treatment and fluoroalkyl silane self-assembly
Li et al. Study of water repellency and corrosion of STA-PFOA modified mortar
CN104789021A (en) Organic-inorganic composite anti-corrosion coating resisting to medium-high temperature geothermal environments, and preparation method for coating
CN108456878B (en) A kind of nano grain surface Modified lift conversion film performance methodology
Lv et al. Synergistically assembled graphene/ZnO composite to enhance anticorrosion performance of waterborne epoxy coatings
CN105969034A (en) Anti-contamination metal copper anticorrosive coating and preparing method thereof
Wu et al. Preparation of epoxy/ZrO 2 composite coating on the Q235 surface by electrostatic spraying and its corrosion resistance in 3.5% NaCl solution
Rahimi et al. Anticorrosive interfacial coatings for metallic substrates
Li et al. Effect of heating self-healing and construction of composite structure on corrosion resistance of superhydrophobic phosphate ceramic coating in long-term water environment
Xie et al. Long-lasting anti-corrosion of superhydrophobic coating by synergistic modification of graphene oxide with polydopamine and cerium oxide
Liu et al. Fabricating Superhydrophobic Protective Films with Enhanced Self‐Cleaning and Anti‐Corrosion Properties through Multiple Anodic Oxidations on Aluminum Alloys
CN109183131B (en) SiO (silicon dioxide)2Preparation method of base composite super-hydrophobic metal surface
KR20130117407A (en) Fabrication method of anti-alkalinity coating layer
CN109355648A (en) In the method that copper alloy surface prepares based superhydrophobic thin films
CN107974143B (en) Corrosion-resistant glass flake resin
CN113462282B (en) Marine anticorrosive oil-repellent coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20200925

WD01 Invention patent application deemed withdrawn after publication