CN108659675B - Preparation method of long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride - Google Patents
Preparation method of long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride Download PDFInfo
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- CN108659675B CN108659675B CN201810498821.0A CN201810498821A CN108659675B CN 108659675 B CN108659675 B CN 108659675B CN 201810498821 A CN201810498821 A CN 201810498821A CN 108659675 B CN108659675 B CN 108659675B
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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
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- 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
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Abstract
The invention discloses a preparation method of an epoxy resin-based long-acting corrosion-resistant wave-transmitting coating. The components of the invention comprise the following components in parts by mass: 80-100 parts of epoxy resin, 20-50 parts of curing agent, 10-40 parts of solvent, 1-10 parts of modified silicon nitride and 1-10 parts of modified graphene. In the invention, the modified filler has good dispersibility in epoxy resin and simultaneously shows certain wave-transmitting performance, and after the test on the dielectric constant and the dielectric loss tangent value of the coating, the wave-transmitting performance of the coating can reach the standard of a commercial wave-transmitting material, and the dielectric constant is 3.42. The composite coating has high density and strong adhesive force, and ensures the corrosion protection of the coating on the carbon steel substrate while transmitting waves. The experiment is simple to operate, obvious in effect and wide in application prospect.
Description
Technical Field
The invention relates to the technical field of organic coatings, in particular to a preparation method of a long-acting corrosion-resistant wave-transparent coating.
Background
With the development of marine technology, the demand for high-speed accurate guidance of ships and marine instruments is increasing. In order to ensure that an antenna system inside a radar or missile can normally work in a high-temperature flying environment and protect antenna tuning radiation from interference, an antenna window and an antenna housing are required to have wave-transmitting performance coupled with the use frequency of an aircraft radar antenna, minimum insertion loss and the like. In addition, the sea mainly contains sodium chloride, and metal materials are more easily corroded in the sea. Meanwhile, the physical properties of the material, such as electricity, optics and the like, are reduced, and the service life of the equipment is shortened. Therefore, the research on the protection of the metal material in seawater is very important.
Chinese patent CN100422114C discloses a high-strength silicon nitride porous ceramic wave-transmitting material for aerospace and a preparation method thereof, wherein a wave-transmitting coating is prepared by mixing silicon nitride, rare earth oxide and a pore-forming agent, and the high-strength silicon nitride porous ceramic wave-transmitting material has a good wave-transmitting effect. However, this method requires high-temperature sintering, thermal spraying, etc., and is prone to waste of energy, environmental pollution, and increased cost.
Chinese patent CN104059601B discloses a method for synthesizing a phosphate wave-transmitting material, which is prepared by mixing inorganic adhesive, template agent, organic resin and the like, and the phosphate wave-transmitting material has excellent high temperature resistance and wave-transmitting performance. However, this method requires flattening the material every 1 hour and finally requires high temperature firing, which is a complicated process.
The invention aims to overcome the defects of complex process, high pollution, high energy loss, high cost and the like in the preparation process of the traditional wave-transmitting material, and the problem to be solved by the industry is urgently needed.
Disclosure of Invention
The invention aims to develop a long-acting corrosion-resistant wave-transmitting coating based on epoxy resin, which overcomes the defects of high dielectric constant and dielectric loss and poor wave-transmitting performance of the epoxy resin by adding a filler, reduces the dielectric constant and dielectric loss of the epoxy resin, improves the wave-transmitting rate of the epoxy resin, and ensures that the composite coating and a substrate have good adhesive force and long-acting corrosion resistance by using the epoxy resin.
A preparation method of a filler in a long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride is characterized by comprising the following steps: dispersing a proper amount of silicon nitride in a silane coupling agent, ultrasonically vibrating, adjusting the pH value, finally stirring the mixture, centrifuging and drying to obtain the modified silicon nitride powder.
A preparation method of a filler in a long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride is characterized by comprising the following steps: and dispersing a proper amount of graphene in a silane coupling agent, heating in a water bath, stirring, washing, filtering and drying to obtain the modified graphene.
A preparation method of a filler in a long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride is characterized by comprising the following steps: adding modified silicon nitride and modified graphene oxide in different proportions into a solvent, performing ultrasonic treatment to form a uniform suspension, heating in a water bath to react, and finally filtering, washing and drying a product to obtain a mixture of the two materials.
A preparation method of a long-acting corrosion-resistant wave-transparent coating of graphene modified silicon nitride is characterized by comprising the following steps: adding a certain amount of epoxy resin and a certain amount of solvent into the modified composite filler, putting the modified composite filler into a ball milling tank, carrying out ball milling in a ball mill, taking out ball milling liquid, adding a proper amount of polyamide curing agent and a proper amount of solvent, uniformly mixing, coating the mixture on a metal matrix, drying, and curing after the solvent is volatilized to obtain the graphene oxide modified silicon nitride coating, wherein the thickness of the coating is controlled to be 100 plus or minus 150 mm.
The invention has the following positive effects:
the preparation process of the graphene modified silicon nitride coating is simple and feasible, and can realize large-scale industrial production, and the modified silicon nitride coating can realize long-acting corrosion-resistant protection on a ship body in a deep sea environment, can realize long-acting protection on an antenna housing, and has better wave-transmitting rate. The prepared modified silicon nitride coating was subjected to electrochemical and adhesion tests in a neutral electrolyte solution of 3.5 wt.% NaCl solution at 100-107And (3) carrying out dielectric property test under an alternating current field of Hz. Contact angle tests show that the coating has good hydrophobicity, and the contact angle is still 98 degrees after the coating is soaked for 20 days; electrochemical (EIS) test results show that the invention can lead the coating to have good corrosion resistance, and the low-frequency impedance of the coating is still 2.67 multiplied by 10 after the coating is soaked in 3.5 wt.% NaCl solution for 3000 hours10 W cm2(ii) a Meanwhile, the coating has larger adhesion and smaller water absorption, and can keep smaller dielectric constant (reduced to 3.42) and dielectric loss tangent value (reduced to 1.17 multiplied by 10)-2）。
Drawings
FIG. 1 is a dielectric spectrum of the coating of example 1 at different frequencies; (a) a dielectric constant; (b) dielectric loss tangent value.
FIG. 2 is a graph of the water contact angle of the coating of example 1; (a) water contact angle plot after 0 d for the inventive coating; (b) water contact angle plot of the inventive coating after 20 d.
FIG. 3 is an impedance spectrum of the coating of example 1 after soaking in a 3.5 wt.% NaCl solution for 1200 hours; (a) bode diagram; (b) nyquist diagram.
FIG. 4 is an impedance spectrum of the coating of example 1 after immersion for 3000 hours in a 3.5 wt.% NaCl solution; (a) bode diagram; (b) nyquist diagram.
Fig. 5 is a graph of the soaking adhesion of the coating of example 1 in a 3.5 wt.% NaCl solution as a function of soaking time.
Detailed Description
The invention is described in detail below with reference to the accompanying drawings by way of specific embodiments so that the advantages and features of the invention may be more readily understood by those skilled in the art, and the scope of the invention may be clearly and clearly defined.
The following test data for wave permeability, corrosion resistance, adhesion and water absorption for each example show that the coatings prepared according to the invention have good properties, both in single properties and in combination.
Example 1:
a first set of coatings was prepared on the surface of Q235 carbon steel.
Pretreating the metal surface of the Q235 carbon steel. The specification of a sample for measuring impedance is 10 multiplied by 3 mm, soldering tin is welded on a copper wire, the other 5 surfaces except the test are sealed by the mixed liquid of epoxy resin and curing agent, after curing and drying, the surface of the metal is sequentially polished by 400#, 800# and 1000# metallographic abrasive paper, and then the ultrasonic treatment is carried out for 10 min by using ethanol.
The specification of a Q235 carbon steel sample with adhesive force is 50 multiplied by 3 mm, the metal surface is polished by 400# and 800# metallographic abrasive paper in sequence, then ultrasonic treatment is carried out for 10 min by using ethanol, and then ball milling is carried out, wherein the rotating speed is controlled at 360 r/min, and the ball milling is carried out for 6 h.
100 parts of epoxy resin (bisphenol A type epoxy resin, the epoxy value is 0.44, new material of Lanxingxi is tin-free tree)Produced by a grease factory), 25 parts of solvent (the mass ratio of xylene to n-butanol is 7: 3), 30 parts of polyamide curing agent (TY-650, Tianjin Yangan chemical plant) and 5 parts of composite material are added and coated on the metal surface treated in the step (2). 30oC drying and curing for 24 h, 60oC, drying and curing for 24 hours, and controlling the film thickness to be 100 +/-20 mm.
Example 2:
a second set of coatings was prepared on the surface of Q235 carbon steel.
Pretreating the metal surface of the Q235 carbon steel. The specification of a sample for measuring impedance is 10 multiplied by 3 mm, soldering tin is welded on a copper wire, the other 5 surfaces except the test are sealed by the mixed liquid of epoxy resin and curing agent, after curing and drying, the surface of the metal is sequentially polished by 400#, 800# and 1000# metallographic abrasive paper, and then the ultrasonic treatment is carried out for 10 min by using ethanol.
The specification of a Q235 carbon steel sample with adhesive force is 50 multiplied by 3 mm, the metal surface is polished by 400# and 800# metallographic abrasive paper in sequence, then ultrasonic treatment is carried out for 10 min by using ethanol, and then ball milling is carried out, wherein the rotating speed is controlled at 300 r/min, and the ball milling is carried out for 6 h.
100 parts of epoxy resin (bisphenol A epoxy resin, epoxy value of 0.44, produced by a Caesalpinia crista new material tin-free resin factory), 25 parts of solvent (the mass ratio of xylene to n-butyl alcohol is 7: 3), 30 parts of polyamide curing agent (TY-650, Tianjin Yangan chemical plant) and 2 parts of composite material are added, and the mixture is coated on the metal surface treated in the step (2). 30oC drying and curing for 24 h, 60oC, drying and curing for 24 h, and controlling the film thickness to be 150 +/-20 mm.
Example 3:
a third set of coatings was prepared on the surface of Q235 carbon steel.
Pretreating the metal surface of the Q235 carbon steel. The specification of a sample for measuring impedance is 10 multiplied by 3 mm, soldering tin is welded on a copper wire, the other 5 surfaces except the test are sealed by the mixed liquid of epoxy resin and curing agent, after curing and drying, the surface of the metal is sequentially polished by 400#, 800# and 1000# metallographic abrasive paper, and then the ultrasonic treatment is carried out for 10 min by using ethanol.
The specification of a Q235 carbon steel sample with adhesive force is 50 multiplied by 3 mm, the metal surface is polished by 400# and 800# metallographic abrasive paper in sequence, then ultrasonic treatment is carried out for 10 min by using ethanol, and then ball milling is carried out, wherein the rotating speed is controlled at 360 r/min, and the ball milling is carried out for 6 h.
100 parts of epoxy resin (bisphenol A epoxy resin, epoxy value of 0.44, produced by a Caesalpinia crista new material tin-free resin factory), 25 parts of solvent (the mass ratio of xylene to n-butyl alcohol is 7: 3), 30 parts of polyamide curing agent (TY-650, Tianjin Yangan chemical plant) and 5 parts of composite material are added, and the mixture is coated on the metal surface treated in the step (2). 30oC, drying and curing for 20 h, 60oC, drying and curing for 8 h, and controlling the film thickness to be 150 +/-20 mm.
Example 4:
and preparing a fourth group of coatings on the surface of the Q235 carbon steel.
Pretreating the metal surface of the Q235 carbon steel. The specification of a sample for measuring impedance is 10 multiplied by 3 mm, soldering tin is welded on a copper wire, the other 5 surfaces except the test are sealed by the mixed liquid of epoxy resin and curing agent, after curing and drying, the surface of the metal is sequentially polished by 400#, 800# and 1000# metallographic abrasive paper, and then the ultrasonic treatment is carried out for 10 min by using ethanol.
The specification of a Q235 carbon steel sample with adhesive force is 50 multiplied by 3 mm, the metal surface is polished by 400# and 800# metallographic abrasive paper in sequence, then ultrasonic treatment is carried out for 10 min by using ethanol, and then ball milling is carried out, wherein the rotating speed is controlled at 200 r/min, and the ball milling is carried out for 6 h.
100 parts of epoxy resin (bisphenol A epoxy resin, epoxy value of 0.44, produced by a Caesalpinia crista new material tin-free resin factory), 25 parts of solvent (the mass ratio of xylene to n-butyl alcohol is 7: 3), 30 parts of polyamide curing agent (TY-650, Tianjin Yangan chemical plant) and 5 parts of composite material are added, and the mixture is coated on the metal surface treated in the step (2). 30oC, drying and curing for 20 h, 60oC, drying and curing for 24 h, and controlling the film thickness to be 130 +/-20 mm.
Claims (4)
1. A preparation method of a graphene modified silicon nitride long-acting corrosion-resistant wave-transparent coating is characterized by comprising the following steps: the components comprise the following components in parts by mass: 80-100 parts of epoxy resin, 20-50 parts of curing agent, 10-40 parts of solvent, 1-10 parts of modified silicon nitride and 1-10 parts of modified graphene; the modified graphene is a grafting product of single-layer or few-layer graphene and a silane coupling agent; the modified silicon nitride is a grafted product of silicon nitride powder and a silane coupling agent;
will modify Si3N4Adding the powder and the modified graphene powder into N, N-dimethylformamide, carrying out ultrasonic treatment to form a uniform suspension, reacting at a high temperature, and filtering, washing and drying a product to obtain a modified mixture;
the preparation method of the coating comprises the following steps: adding the modified mixture into epoxy resin and a solvent, then placing the mixture into a ball milling tank, carrying out ball milling in a ball mill, then taking out ball milling liquid, adding a curing agent and the solvent, uniformly mixing, coating on a metal matrix, drying and curing to obtain the graphene modified silicon nitride coating.
2. The preparation method of the graphene-modified silicon nitride long-acting corrosion-resistant wave-transmitting coating according to claim 1, characterized by comprising the following steps: the epoxy resin is bisphenol A epoxy resin.
3. The preparation method of the graphene-modified silicon nitride long-acting corrosion-resistant wave-transmitting coating according to claim 1, characterized by comprising the following steps: the curing agent is a low molecular polyamide curing agent.
4. The preparation method of the graphene-modified silicon nitride long-acting corrosion-resistant wave-transmitting coating according to claim 1, characterized by comprising the following steps: the solvent is one or a mixture of xylene and n-butanol in any proportion.
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| CN112500760B (en) * | 2020-06-04 | 2021-12-10 | 中国海洋大学 | polyaniline/MOF composite coating electrode material, and preparation method and application thereof |
| CN113637380B (en) * | 2021-08-27 | 2022-07-05 | 武汉理工大学 | Preparation method of graphene oxide-silicon nitride composite powder/urushiol formal composite coating |
| CN115847987B (en) * | 2022-12-02 | 2023-12-08 | 苏州铂韬新材料科技有限公司 | Film material with wave-transmitting and heat-conducting functions and preparation process thereof |
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| US20150125646A1 (en) * | 2013-11-05 | 2015-05-07 | Espci Innov | Self-Healing Thermally Conductive Polymer Materials |
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| KR101405322B1 (en) * | 2014-02-28 | 2014-06-11 | 부림산업개발(주) | Inorganic ceramic paint for curing at room temperature and painting method using the same |
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