CN115386279A - Fluorine-containing acrylate hydrophobic anticorrosive coating and preparation method thereof - Google Patents

Fluorine-containing acrylate hydrophobic anticorrosive coating and preparation method thereof Download PDF

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Publication number
CN115386279A
CN115386279A CN202210966696.8A CN202210966696A CN115386279A CN 115386279 A CN115386279 A CN 115386279A CN 202210966696 A CN202210966696 A CN 202210966696A CN 115386279 A CN115386279 A CN 115386279A
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China
Prior art keywords
fluorine
coating
containing acrylate
hydrophobic
fluoroacrylate
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CN202210966696.8A
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Chinese (zh)
Inventor
易昌凤
曾凡宝
徐祖顺
纪浩南
霍亚楠
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Hubei University
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Hubei University
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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
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular

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

Abstract

The invention discloses a fluorine-containing acrylate hydrophobic anticorrosion coating, which consists of 100 parts by mass of epoxy resin, 5-20 parts by mass of fluorine-containing acrylate and 5 parts by mass of epoxy curing agent; the fluorine-containing acrylate is a binary block polymer which is polymerized by taking hexafluorobutyl methacrylate and glycidyl methacrylate as main raw materials and adding an initiator, a catalyst and a coordination agent. The invention also discloses a preparation method of the fluorine-containing acrylate hydrophobic anticorrosive coating. The fluorine-containing acrylate hydrophobic anticorrosive coating prepared by adjusting the feed ratio of the raw materials and utilizing the interaction relationship among the groups has the dual properties of high mechanical strength and corrosion resistance, does not generate tiny cracks even being used for a long time, and greatly prolongs the service life of the anticorrosive coating; the binary block polymer fluorine-containing acrylate is synthesized under the nitrogen condition, a reducing agent is not required to be added in the reaction, and the method is environment-friendly and harmless.

Description

Fluorine-containing acrylate hydrophobic anticorrosive coating and preparation method thereof
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a fluorine-containing acrylate hydrophobic anticorrosive coating and a preparation method thereof.
Background
Coatings are known as a material for protecting the surface of a substrate, and as a functional material, a coating can be applied to the surface of the substrate by various molding processes to form a solid film, wherein especially, the hydrophobic anticorrosion coating is notable for having surface specific wettability and can be applied in many fields, and is in the recent years, for example: self-cleaning, anti-icing, anti-fogging, reduced drag, etc. However, with the continuous progress of science and technology, the traditional acrylate coating is difficult to meet the requirements of people, and the hydrophobic coating which is more corrosion-resistant and higher in strength has a wide market prospect.
After the coating is formed on the substrate material, the existing acrylate coating has low strength and short service life, and the anticorrosive effect is difficult to meet the requirements of people. Along with long-time use, the coating surface can appear the crack, and the crack can lead to corroding the medium invasion coating to lead to the coating to lose the guard action, coating crack or infiltration phenomenon are difficult to discover, lead to protecting the substrate by the corruption, seriously influence anticorrosive coating life. Moreover, conventional acrylate coatings require the use of reducing agents during the manufacturing process, and most reducing agents are relatively toxic. In addition, most methods for preparing the hydrophobic anticorrosive coating at present have complex process and high cost, and limit the development of the methods.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention aims to prepare the hydrophobic anticorrosive coating with good anticorrosive effect, high strength and long service life.
In order to achieve the above object, according to one aspect of the present invention, there is provided a fluorine-containing acrylate hydrophobic anticorrosion coating, comprising 100 parts by mass of an epoxy resin, 5 to 20 parts by mass of a fluorine-containing acrylate, and 5 parts by mass of an epoxy hardener; the fluorine-containing acrylate is a binary block polymer which is polymerized by taking hexafluorobutyl methacrylate and glycidyl methacrylate as main raw materials and adding an initiator, a catalyst and a coordination agent.
Further, the mass ratio of the hexafluorobutyl methacrylate to the glycidyl methacrylate is 20:7.
further, the initiator is ethyl 2-bromoisobutyrate.
Further, the catalyst is copper bromide.
Further, the complexing agent is pentamethyldiethylenetriamine.
Further, the epoxy curing agent is polyamide 650.
According to another aspect of the invention, a preparation method of the fluorine-containing acrylate hydrophobic anticorrosion coating is provided, which comprises the following steps:
s100: adding hexafluorobutyl methacrylate into a reaction vessel, stirring, adding glycidyl methacrylate, an initiator, a catalyst and a coordination agent, and reacting under the nitrogen condition to obtain binary block polymer fluorine-containing acrylate;
s200: and adding fluorine-containing acrylate into the epoxy resin, stirring, adding an epoxy curing agent, uniformly stirring, coating on a base material, and drying to obtain the hydrophobic anticorrosive coating.
Further, the nitrogen condition in S100 is to introduce nitrogen into the reaction vessel for 5min.
Further, the reaction described in S100 was carried out at 80 ℃ for 2h.
Further, the drying condition of S200 is drying for 3h at 50 ℃.
Compared with the prior art, the invention can obtain the following beneficial effects:
the fluorine-containing acrylate hydrophobic anticorrosive coating prepared by adjusting the feed ratio of the raw materials and utilizing the interaction relationship among the groups has the dual properties of high mechanical strength and corrosion resistance, does not generate tiny cracks even being used for a long time, and greatly prolongs the service life of the anticorrosive coating; the binary block polymer fluorine-containing acrylate is synthesized under the nitrogen condition, a reducing agent is not required to be added in the reaction, the method is environment-friendly and harmless, and the prepared coating has wide application prospects in the fields of self-cleaning, ice resistance, fog resistance and the like. Meanwhile, the invention adopts one-pot method free radical polymerization to synthesize fluorine-containing acrylate, and has simple operation and low cost.
Drawings
FIG. 1 is an infrared spectrum of a fluoroacrylate in an example of the present invention;
FIG. 2 is a graph of impedance curve analysis of a hydrophobic corrosion protection coating in an example of the present invention;
FIG. 3 is an analysis graph of the impedance curve of the hydrophobic anti-corrosion coating in an example of the invention after soaking in 3.5% NaCl solution for 20 days.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a hydrophobic anti-corrosion coating containing fluoroacrylate, which consists of 100 parts by mass of epoxy resin, 5-20 parts by mass of fluoroacrylate (PFEMA) and 5 parts by mass of epoxy curing agent polyamide 650; wherein the fluorine-containing acrylate (PFEMA) is prepared by mixing the following components in a mass ratio of 20:7 hexafluorobutyl methacrylate (HFBMA) and Glycidyl Methacrylate (GMA) are taken as main raw materials, and initiator 2-bromoethyl isobutyrate, catalyst copper bromide and coordination agent pentamethyldiethylenetriamine are added for polymerization to form a binary block polymer.
The invention also provides a preparation method of the fluorine-containing acrylate hydrophobic anticorrosive coating, which comprises the following steps:
s100: adding hexafluorobutyl methacrylate (HFBMA) into a reaction vessel, stirring, adding Glycidyl Methacrylate (GMA), an initiator ethyl 2-bromoisobutyrate, a catalyst copper bromide and a complexing agent pentamethyldiethylenetriamine, introducing nitrogen for 5min, and reacting for 2h at 80 ℃ to obtain binary block polymer fluorine-containing acrylate (PFEMA);
s200: adding fluorine-containing acrylate (PFEMA) into epoxy resin, stirring, adding epoxy curing agent polyamide 650, uniformly stirring, coating on a base material, and drying in an oven at 50 ℃ for 3 hours to obtain the hydrophobic anticorrosive coating.
Example 1
A250 ml four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser, a drying tube and a nitrogen inlet was charged with 10.0g of water-removed hexafluorobutyl methacrylate (HFBMA), and after stirring, 3.5g of Glycidyl Methacrylate (GMA), 0.2g of ethyl 2-bromoisobutyrate (EBiB) and 0.003g of copper bromide (CuBr) were added 2 ) 0.03g of Pentamethyldiethylenetriamine (PMDETA), introducing nitrogen for 5min, and reacting at 80 ℃ for 2h to obtain the diblock polymer fluorine-containing acrylate (PFEMA).
FIG. 1 is an infrared spectrum of PFEMA, 2986cm as shown in FIG. 1 -1 is-CH 3 A stretching vibration peak; 1734cm -1 Is the stretching vibration peak of C = O; 1446cm -1 And 1930cm -1 is-CH 2 The stretching vibration peak of (1); 1255cm -1 And 1168cm -1 Are respectively corresponding to-CF 3 ，—CF 2 The bending vibration peak of (1); 958cm -1 An epoxy characteristic peak of GMA; furthermore, at 1600cm -1 The nearby peak disappeared, indicating that group C = C has reacted to completion, also indicating successful synthesis of PFEMA.
Example 2
Adding 10.0g of epoxy resin into a glass container, stirring for 10min by using a glass rod, adding 6500.5g of epoxy curing agent polyamide, stirring for 20min, uniformly mixing, blade-coating on tinplate, and then placing in an oven at 50 ℃ for 3h to obtain the hydrophobic anticorrosive coating, wherein the label is PFEMA-0.
Example 3
Adding 10.0g of epoxy resin and 0.5g of PFEMA into a glass container, stirring for 10min by using a glass rod, adding 650.5 g of epoxy curing agent polyamide, stirring for 20min, after uniform mixing, blade-coating on tinplate, and then placing in an oven at 50 ℃ for 3h to obtain the hydrophobic anticorrosive coating, wherein the label is PFEMA-1.
Example 4
Adding 10.0g of epoxy resin and 1g of PFEMA into a glass container, stirring for 10min by using a glass rod, adding 650.5 g of epoxy curing agent polyamide, stirring for 20min, after mixing uniformly, blade-coating on tinplate, and then placing in an oven at 50 ℃ for 3h to obtain a hydrophobic anticorrosive coating, wherein the label is PFEMA-2.
Example 5
Adding 10.0g of epoxy resin and 1.5g of PFEMA into a glass container, stirring for 10min by using a glass rod, adding 650.5 g of epoxy curing agent polyamide, stirring for 20min, after uniform mixing, blade-coating on tinplate, and then placing in an oven at 50 ℃ for 3h to obtain a hydrophobic anticorrosive coating, wherein the label is PFEMA-3.
Example 6
Adding 10.0g of epoxy resin and 2g of PFEMA into a glass container, stirring for 10min by using a glass rod, adding 650.5 g of epoxy curing agent polyamide, stirring for 20min, after mixing uniformly, blade-coating on tinplate, and then placing in an oven at 50 ℃ for 3h to obtain a hydrophobic anticorrosive coating, wherein the label is PFEMA-4.
Comparative analysis of the hydrophobic properties of the hydrophobic corrosion protection coatings prepared in examples 2-6:
the Water Contact Angle (WCA) of the hydrophobic anticorrosion coating is shown in the following table, and as can be seen from the table, the prepared PFEMA hydrophobic anticorrosion coating has the best effect of PFEMA-4, the contact angle reaches 121 degrees, and excellent hydrophobic performance is shown, so that the optimal coating sample is PFEMA-4.
Sample name PFEMA-0 PFEMA-1 PFEMA-2 PFEMA-3 PFEMA-4
Contact Angle number/° 75 92 109 117 121
Electrochemical Impedance Spectroscopy (EIS) is an important indicator for evaluating the corrosion resistance of a coating, and the corrosion resistance of a PFEMA hydrophobic corrosion-resistant coating can be compared by analyzing the impedance curve of the PFEMA hydrophobic corrosion-resistant coating.
Fig. 2 is an impedance curve analysis diagram of the hydrophobic anticorrosion coating, and it can be seen from fig. 2 that the impedance arc and the impedance value of the sample with PFEMA added are better than those of the coating without PFEMA added, and as the amount of PFEMA increases, the anticorrosion effect of the sample increases and then decreases, which indicates that the anticorrosion effect of the coating is affected by excessive PFEMA added.
FIG. 3 is an analysis graph of the impedance curve of the hydrophobic anticorrosion coating after 20 days of immersion in 3.5% NaCl solution, and as shown in FIG. 3, the samples of PFEMA showed a decrease in both the arc and the value of the impedance after 20 days of immersion in 3.5% NaCl solution due to the immersion of the corrosive medium into the coating and the corrosion of the coating by the corrosive medium. It can also be seen that PFEMA-3 has the best preservative effect after 20 days of soaking. The PFEMA coating still shows excellent corrosion resistance even under the soaking of a corrosion medium for a long time, and the reasons are that the coating has high strength, is compact and has low surface energy to effectively block the corrosion medium. Therefore, the prepared PFEMA coating has good corrosion prevention effect and long service life, and has wide prospect in the fields of corrosion prevention and the like.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A fluorine-containing acrylate hydrophobic anticorrosion coating is characterized in that: the coating consists of 100 parts by mass of epoxy resin, 5-20 parts by mass of fluorine-containing acrylate and 5 parts by mass of epoxy curing agent; the fluorine-containing acrylate is a binary block polymer which is polymerized by taking hexafluorobutyl methacrylate and glycidyl methacrylate as main raw materials and adding an initiator, a catalyst and a coordination agent.
2. The fluoroacrylate hydrophobic corrosion protection coating of claim 1, wherein: the mass ratio of the hexafluorobutyl methacrylate to the glycidyl methacrylate is 20:7.
3. the fluoroacrylate hydrophobic corrosion protection coating of claim 1, wherein: the initiator is 2-bromoisobutyric acid ethyl ester.
4. The fluoroacrylate hydrophobic corrosion protection coating of claim 1, wherein: the catalyst is copper bromide.
5. The fluoroacrylate hydrophobic corrosion protection coating of claim 1, wherein: the complexing agent is pentamethyl diethylenetriamine.
6. The fluoroacrylate hydrophobic corrosion protection coating of claim 1, wherein: the epoxy curing agent is polyamide 650.
7. A method for preparing the hydrophobic corrosion protection coating containing fluoroacrylate according to any one of claims 1 to 6, wherein the method comprises the steps of:
s100: adding hexafluorobutyl methacrylate into a reaction vessel, stirring, adding glycidyl methacrylate, an initiator, a catalyst and a coordination agent, and reacting under the nitrogen condition to obtain binary block polymer fluorine-containing acrylate;
s200: and adding fluorine-containing acrylate into the epoxy resin, stirring, adding an epoxy curing agent, uniformly stirring, coating on a base material, and drying to obtain the hydrophobic anticorrosive coating.
8. The method for preparing the fluorine-containing acrylate hydrophobic anticorrosion coating according to claim 7, wherein the method comprises the following steps: s100 under the nitrogen condition, nitrogen is introduced into the reaction vessel for 5min.
9. The method for preparing the hydrophobic anticorrosion coating containing fluoroacrylate of claim 7, wherein the method comprises the following steps: s100 the reaction is carried out at 80 ℃ for 2h.
10. The method for preparing the fluorine-containing acrylate hydrophobic anticorrosion coating according to claim 7, wherein the method comprises the following steps: s200, drying for 3 hours at 50 ℃.
CN202210966696.8A 2022-08-12 2022-08-12 Fluorine-containing acrylate hydrophobic anticorrosive coating and preparation method thereof Pending CN115386279A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104448712A (en) * 2014-12-24 2015-03-25 中科院广州化学有限公司 Organic fluorine modified epoxy LED packaging material and preparation method thereof
CN106867359A (en) * 2017-01-20 2017-06-20 常州大学 A kind of weather-proof anti-corrosion self stratifying coating of fluorine-containing block propylene acid esters epoxy resin and preparation method thereof
CN112831241A (en) * 2021-02-18 2021-05-25 华东理工大学 Super-hydrophobic and super-oleophobic epoxy resin coating and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104448712A (en) * 2014-12-24 2015-03-25 中科院广州化学有限公司 Organic fluorine modified epoxy LED packaging material and preparation method thereof
CN106867359A (en) * 2017-01-20 2017-06-20 常州大学 A kind of weather-proof anti-corrosion self stratifying coating of fluorine-containing block propylene acid esters epoxy resin and preparation method thereof
CN112831241A (en) * 2021-02-18 2021-05-25 华东理工大学 Super-hydrophobic and super-oleophobic epoxy resin coating and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YINWEN LI等: "Synthesis of fluorinated block copolymer and superhydrophobic cotton fabrics preparation", PROGRESS IN ORGANIC COATINGS/SYNTHESIS OF FLUORINATED BLOCK COPOLYMER AND SUPERHYDROPHOBIC COTTON FABRICS PREPARATION *

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