CN107793888A - A kind of anti-corrosion nano MoS2The preparation method of RGO epoxy composite coatings - Google Patents

A kind of anti-corrosion nano MoS2The preparation method of RGO epoxy composite coatings Download PDF

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CN107793888A
CN107793888A CN201711067566.6A CN201711067566A CN107793888A CN 107793888 A CN107793888 A CN 107793888A CN 201711067566 A CN201711067566 A CN 201711067566A CN 107793888 A CN107793888 A CN 107793888A
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mos
rgo
preparation
corrosion resistant
composite coatings
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CN107793888B (en
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陈春林
何毅
肖国清
夏云卿
何�泽
伍友清
李虹杰
钟菲
石恒
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Chengdu Heng Gu New Mstar Technology Ltd
Daqing Baoyi Petroleum Technology Co ltd
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Southwest Petroleum 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
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers

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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)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a kind of corrosion resistant nanometer MoS2RGO epoxy composite coatings, its preparation method comprise the following steps：（1）The preparation of base-material；（2 two-dimentional MoS2The preparation of RGO nano-hybrid materials；（3）Modified two-dimentional MoS2The preparation of RGO nano-hybrid materials；（4）Corrosion resistant nanometer MoS2The preparation of RGO epoxy composite coatings：Weigh base-material, modified two-dimentional MoS2RGO nano-hybrid materials, mixing, ultrasonic disperse 30min, dispersed system is formed, then moves it into spray gun, rectangle steel disc of the high pressure painting surface through blasting treatment, after the completion of spraying, normal temperature cure 7 days, obtains corrosion resistant nanometer MoS2RGO epoxy composite coatings.In preparation process, after loading molybdenum disulfide on graphene oxide, surface of graphene oxide energy on the one hand can be effectively reduced, improves the dispersiveness of graphene oxide.On the other hand the MoS prepared2RGO nano-hybrid materials can effectively improve composite coating and stop that corrosive medium enters substrate performance, so as to improve the decay resistance of composite coating, osmotic-pressure-tolerant.

Description

A kind of anti-corrosion nano MoS2The preparation method of-RGO- epoxy composite coatings
Technical field
The invention belongs to the preparation method field of epoxy nano composite material, and in particular to a kind of corrosion resistant nanometer MoS2The preparation method of-RGO- epoxy composite coatings.
Background technology
Epoxy resin after solidification（EP）With good physics, chemical property, it is to metal and the table of nonmetallic materials Face has excellent adhesion strength, and dielectric properties are good, and set shrinkage factor is small, and hardness is high, and pliability is preferable, to alkali and major part Solvent-stable.But single epoxy coating but faces a severe challenge in severe corrosive environment.It is but nano combined The Corrosion Protection of coating is but much better than single resinous coat.And the blocking effect of composite coating is to corrosion resistance and thermostabilization Property to close weight.Therefore, we usually introduce the nano structural material with layer structure to improve the barrier property of coating.Graphite Olefinic oxide（GO）, a kind of interesting two dimension of novelty（2D）Carbon nanomaterial, the interest of various fields is caused.Widely Research shows that graphene-based coating is the excellent anti-corrosion barrier of metal.Can be due to their high surface area and strong Van der Waals Power, GO lamellas are easily reunited together, thus limit their further applying in the polymer.Therefore, researcher does Many effort reduce its agglomeration, a kind of simple effective method be exactly in its surface load one layer of nano material with Improve its in the polymer scattered.
Two-dimentional MoS2Layer is stacked by the interaction of Van der Waals force and formed, and has the desirable properties similar to graphene. But the work largely reported lays particular emphasis on MoS2Application in the field such as catalysis/electronics and lubricating oil, almost not anti- Application in terms of rotten coating.But MoS2It is still far from perfect in the research of corrosion field.So we are by nanometer MoS2Lamella loads To GO surface, two-dimentional MoS is obtained2- RGO hybrid materials, then by nanometer MoS2- RGO hybrid materials are dispersed in epoxy resin In, to improve corrosion resistance and heat endurance.
The content of the invention
The corrosion resistant nanometer MoS that the present invention provides for above-mentioned weak point2The preparation of-RGO- epoxy composite coatings Method, and opened up nanometer MoS2Application of-RGO the hybrid materials in corrosion-inhibiting coating field.The process is by hydro-thermal method by MoS2Receive Rice grain is equably supported on GO surfaces, and use γ-（2,3- glycidoxies）Propyl trimethoxy silicane（KH560）It is right It is modified.Modified MoS2- RGO hybrid materials are combined with epoxy resin, prepare corrosion resistant nanometer MoS2- RGO- epoxies Composite coating.
To achieve the above object, the technical solution adopted for the present invention to solve the technical problems is.
A kind of corrosion resistant nanometer MoS2The preparation method of-RGO- epoxy composite coatings, comprises the following steps：（1）Base-material Preparation
Epoxy resin, curing agent, acetone mixing are weighed, 300r/min is stirred 6 days, and then 60r/min stirrings 1 day, are obtained uniformly The base-material of mixing.
（2）Two-dimentional MoS2The preparation of-RGO nano-hybrid materials.
0.5g GO are added in 30ml deionized waters, swung 1 hour by ultrasound cleaner vibrator.Then by the secondary molybdenums of 1g Sour ammonium and 1.5g thiocarbamide is added in GO solution, and continues to be stirred vigorously 2h.Mixed solution will be stirred and pour into hydrothermal reactor In, and reacted 16 hours at 220 DEG C.Reaction product is washed 3 times with ethanol and deionized water mixed solution.Finally by MoS2- RGO nano-hybrid materials are dried in 333.15K vacuum drying oven.
（3）Two-dimentional MoS2The modification of-RGO nano-hybrid materials.
Weigh 1g MoS2- RGO nano-hybrid materials are added to containing in deionized water/alcohol mixed solution beaker.And Ultrasonic disperse 30 minutes in numerical control ultrasonic cleaner.Then 0.05g KH560 are added into beaker.After vibration shakes up, by before Solution is stated to be transferred in three-necked flask.Then stirring reaction vacuum filter, drying after 8 hours under 85 DEG C of water-baths.
（4）Corrosion resistant nanometer MoS2The preparation of-RGO- epoxy composite coatings.
Weigh base-material, modified MoS2- RGO nano-hybrid materials, mixing, ultrasonic disperse 30min, form homogeneous dispersion System, then dispersed system is moved into spray gun, rectangle steel disc of the high pressure painting surface through blasting treatment, spraying is completed Afterwards, normal temperature cure 7 days, corrosion resistant nanometer MoS is obtained2- RGO- epoxy composite coatings.
Further, step（1）Epoxy resin, curing agent, the weight ratio of acetone are 3-4：1:3-4.
Further, step（1）Middle curing agent is ethylenediamine, diethylenetriamine, triethylene tetramine.
Further, step（4）Middle modified MoS2- RGO nano-hybrid materials account for the 1wt% of system gross mass.
A kind of corrosion resistant nanometer MoS provided by the invention2The preparation of-RGO- epoxy composite coatings, have beneficial below Effect.
（1）The epoxy composite coating belongs to air-curing coatings, and preparation process simple possible, cost is low, suitable for industry Metaplasia is produced.
（2）The MoS prepared2- RGO- epoxy composite coatings, after loading molybdenum disulfide on graphene oxide, a side Face can effectively reduce surface of graphene oxide energy, improve the dispersiveness of graphene oxide.On the other hand the two dimension prepared Hybrid material can effectively improve the barrier properties of composite coating, so as to improve corrosion-resistant, the osmotic-pressure-tolerant energy of composite coating.
Brief description of the drawings
Fig. 1 is MoS2It is 1 with GO ratios:1 scanning electron microscope (SEM) photograph.
Fig. 2 is MoS2It is 1 with GO ratios:2 scanning electron microscope (SEM) photograph.
Fig. 3 is MoS2It is 1 with GO ratios:4 scanning electron microscope (SEM) photograph.
Fig. 4 is MoS2It is 1.5 with GO ratios:1 scanning electron microscope (SEM) photograph.
Fig. 5 is MoS2Transmission electron microscope picture.
Fig. 6 is MoS2- RGO hybrid material transmission electron microscope pictures.
Fig. 7 is the Nyquists figures that different nano-composite coatings impregnate composite coating after 120h in 3.5%NaCl solution.
Fig. 8 is that different nano-composite coatings soak the polarization curve after 2h.
Fig. 9 is the contact angle figure before and after different nano-composite coatings soak 5 days in 3.5%NaCl solution；Wherein A is MoS2The contact angle of-RGO/ epoxy coatings；B is the contact angle of GO/ epoxy coatings；C is MoS2/ epoxy coating Contact angle；D is the contact angle of pure epoxy resin coating.
Embodiment
Embodiment 1
A kind of corrosion resistant nanometer MoS2The preparation method of-RGO- epoxy composite coatings, comprises the following steps.
（1）The preparation of base-material.
Weigh the epoxy resin for being ground into fine-powdered（EP）300g, short-chain fat amine hardener 100g and 350g acetone mix Close, 300r/min is stirred 6 days, then 60 r/min stirrings 1 day, the base-material being uniformly mixed；Wherein short-chain fat amine solidifies Agent is ethylenediamine（EDA）, diethylenetriamine（DTA）Or triethylene tetramine（TTA）.
（2）Two-dimentional MoS2The preparation of-RGO nano-hybrid materials.
0.05gGO is added in 30ml deionized waters, swung 1 hour by ultrasound cleaner vibrator.Then it is 0.1g is secondary Ammonium molybdate and 0.15g thiocarbamides are added in GO solution, and continue to be stirred vigorously 2h.Mixed solution will be stirred and pour into hydro-thermal reaction In device, and reacted 16 hours at 220 DEG C.Reaction product is washed 3 times with ethanol and deionized water mixed solution.Finally will MoS2- RGO nano-hybrid materials are dried in 333.15K vacuum drying oven.
（3）Two-dimentional MoS2The modification of-RGO nano-hybrid materials.
Weigh 1g MoS2- RGO nano-hybrid materials are added to containing in deionized water/alcohol mixed solution beaker.And Ultrasonic disperse 30 minutes in numerical control ultrasonic cleaner.Then 0.05g KH560 are added into beaker.After vibration shakes up, by before Solution is stated to be transferred in three-necked flask.Then stirring reaction vacuum filter, drying after 8 hours under 85 DEG C of water-baths.
（4）Corrosion resistant nanometer MoS2The preparation of-RGO- epoxy composite coatings.
Weigh base-material, modified MoS2- RGO nano-hybrid materials, mixing, ultrasonic disperse 30min, form homogeneous dispersion System, then dispersed system is moved into spray gun, rectangle steel disc of the high pressure painting surface through blasting treatment, spraying is completed Afterwards, normal temperature cure 7 days, corrosion resistant nanometer MoS is obtained2- RGO- epoxy composite coatings.Wherein, base-material, MoS2、GO、MoS2-RGO The ratio for accounting for dispersion gross weight respectively is shown in Table 1.
Experimental example
Respectively by GO, MoS2, modified MoS2- RGO and epoxy resin mixing, ultrasonic disperse 1h, prepare GO, MoS respectively2, it is modified MoS2- RGO contents are 1wt% GO/ epoxy coatings, MoS2/ epoxy coating, MoS2- RGO/ epoxy coatings, The matrix steel disc of even application in spray gun in sandblasting and welding is moved it into respectively（N80）On, coating is sprayed on matrix steel Carried out in 1 hour after the completion of piece blasting treatment, after the completion of spraying, the steel disc of coating solidifies 7 days at normal temperatures, is tried Sample.Control is used as using pure epoxy resin.
（1）The cross-section morphology of each coating is observed using JSM-7500F SEM, as a result sees accompanying drawing 1-4.From figure 3 as can be seen that work as MoS2Dosage ratio with GO is 1:When 4, GO surfaces are hardly visible MoS2Nanometer sheet.As increase MoS2Contain Amount, the dosage ratio for making itself and GO is 1:When 2, the MoS on GO surfaces is should be apparent that from Fig. 22Layer structure, but can not GO surfaces are completely covered.But continue to increase MoS2Dosage ratio with GO is 1:When 1, it will be seen from figure 1 that MoS2Nanometer sheet GO surface can be supported on uniformity and completely.From fig. 4, it can be seen that work as MoS2Dosage ratio with GO is 1.5:When 1, Nanometer MoS2Occurs the phenomenon reunited on GO surfaces.
（2）Using TecnaiG2F20S-TWIN Flied emission transmission electron microscopes（TEM）Observe MoS2And MoS2- RGO is miscellaneous Change the pattern of material, as a result see accompanying drawing 5-6.It can see from Fig. 5,6, MoS2Typical layer structure is showed, and in GO Uniformity loads on surface.Illustrate to work as MoS2Dosage ratio with GO is 1:When 1, MoS2Can uniformly it disperse on GO surfaces. The effect for preventing corrosive medium from entering base material is served, improves the corrosion resistance of coating.
（3）Sample is measured using CS310 electrochemical workstations, as a result sees accompanying drawing 7-8.It is from figure 7 it can be seen that pure Epoxy,（1wt%）MoS2/ epoxy,（1wt%）GO/epoxy and（1wt%）MoS2- RGO/epoxy coating samples are in 3.5%NaCl After soaking 168h in solution, pure epoxy impedances radius is minimum, MoS2- RGO/epoxy coating impedances radius is maximum.Illustrate MoS2- The antiseptic property of RGO/epoxy coatings is much better than other 3 kinds of coatings.Can be with fitting parameter from Fig. 8 polarization curves and table 1 Find out, after immersion 2 hours, MoS2The corrosion electric current density of-RGO/epoxy coatings is respectively less than other several coatings, and explanation changes Property two dimension MoS2The addition of-RGO nano-hybrid materials is favorably improved the antiseptic property of epoxy coating.
（4）Using KRUSS DSA30S interface parameter one measuring system measure material surface contact angle, accompanying drawing is as a result seen 9.The test of contact angle can represent the hydrophobic situation of material interface, and contact angle is bigger, and hydrophobicity is stronger.It can be reflected with side Material prevents the ability that aqueous caustic medium enters coating.It can be seen in figure 9 that MoS2- RGO/epoxy coating surfaces contact Angle is more than pure epoxy,（1wt%）MoS2/ epoxy,（1wt%）GO/epoxy coatings.Illustrate that the hydrophobicity of material is most strong, water-based corruption It is more difficult into coating to lose medium.In addition, after 4 kinds of coatings soak 5 days in 3.5% NaCl solution, all material contact angle There is reduction to show that corrosive medium gradually penetrates into coating.But MoS2- RGO/epoxy contact angle on surface of coating reduces amplitude most It is small, illustrate modified two-dimentional MoS2- RGO nano-hybrid materials can effectively prevent medium from entering coat inside, and antiseptic property obtains To raising.

Claims (4)

  1. A kind of 1. corrosion resistant nanometer MoS2The preparation method of-RGO- epoxy composite coatings, comprises the following steps：
    （1）Two-dimentional MoS2The preparation of-RGO nano-hybrid materials
    0.5g GO are added in 30ml deionized waters, swung 1 hour by ultrasound cleaner vibrator；Then by 1g ammonium paramolybdates It is added to 1.5g thiocarbamides in GO solution, and continues to be stirred vigorously 2h, mixed solution will be stirred and pour into hydrothermal reactor, and Reacted 16 hours at 220 DEG C, reaction product is washed 3 times with ethanol and deionized water mixed solution, finally by MoS2- RGO receives Rice hybrid material is dried in 333.15K vacuum drying oven；
    （3）Two-dimentional MoS2The modification of-RGO nano-hybrid materials
    Weigh 1g MoS2- RGO nano-hybrid materials are added to containing in deionized water/alcohol mixed solution beaker, and in numerical control Ultrasonic disperse 30 minutes in ultrasonic cleaner, 0.05g KH560 are then added into beaker, will be foregoing molten after vibration shakes up Liquid is transferred in three-necked flask, then stirring reaction vacuum filter, drying after 8 hours under 85 DEG C of water-baths；
    （4）Corrosion resistant nanometer MoS2The preparation of-RGO- epoxy composite coatings
    Weigh base-material, modified MoS2- RGO nano-hybrid materials, mixing, ultrasonic disperse 30min, dispersed system is formed, then Dispersed system is moved into spray gun, rectangle steel disc of the high pressure painting surface through blasting treatment, after the completion of spraying, normal temperature Solidification 7 days, obtains corrosion resistant nanometer MoS2- RGO- epoxy composite coatings.
  2. A kind of 2. corrosion resistant nanometer MoS according to claim 12The preparation method of-RGO- epoxy composite coatings, it is special Sign is, step（1）Middle MoS2Dosage with GO is mass ratio 1:1.
  3. A kind of 3. corrosion resistant nanometer MoS according to claim 12The preparation method of-RGO- epoxy composite coatings, it is special Sign is, step（4）Middle MoS2The dosage of-RGO nano-hybrid materials is the 1wt % of system gross mass.
  4. 4. the corrosion resistant nanometer MoS that the method as described in claim any one of 1-4 is prepared2- RGO- epoxy composite coatings.
CN201711067566.6A 2017-11-03 2017-11-03 A kind of anti-corrosion nano MoS2The preparation method of-RGO- epoxy composite coating Active CN107793888B (en)

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CN108753106A (en) * 2018-06-14 2018-11-06 江苏大学 A kind of nano-hybrid material modified epoxy self-lubricating composite coating and preparation method thereof
CN114000133A (en) * 2021-10-22 2022-02-01 江西卓美金属制品有限公司 Zinc steel fence and preparation method thereof
CN115651519A (en) * 2022-12-29 2023-01-31 有研工程技术研究院有限公司 Composite hydrogen permeation resistant coating for hydrogen transmission pipeline and preparation method thereof

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CN108753106A (en) * 2018-06-14 2018-11-06 江苏大学 A kind of nano-hybrid material modified epoxy self-lubricating composite coating and preparation method thereof
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CN115651519A (en) * 2022-12-29 2023-01-31 有研工程技术研究院有限公司 Composite hydrogen permeation resistant coating for hydrogen transmission pipeline and preparation method thereof

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Address after: 611730 Runcheng Garden, 217 Shengli North Street, Deyuan Town, Pidu District, Chengdu City, Sichuan Province, 4 buildings and 2 units

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