CN109909131A - A kind of preparation method of graphene-based steel corrosion-inhibiting coating - Google Patents
A kind of preparation method of graphene-based steel corrosion-inhibiting coating Download PDFInfo
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Abstract
A kind of preparation method of graphene-based steel corrosion-inhibiting coating, the present invention relates to the graphene-based corrosion-inhibiting coating preparation methods that a kind of pair of corrosive medium has excellent isolation and blocking effect.The purpose of the invention is to effectively solve the problems, such as built anticorrosion of steel structure coating antiseptic less effective under high salinity briny environment.Steel surface is carried out degreasing and rust removal and grinding process by the present invention, then one layer of epoxy coating first is coated in the steel surface polished with underwater curing epoxy resin, silane coupling agent, silane coupling agent watersoluble plumbago alkene composite layer, oiliness graphene layer Transition Technology are used again, obtain the excellent corrosion-inhibiting coating of the antiseptic property that can be applied under littoral area, splash zone and high humidity environment, the effect that the graphene-based steel corrosion-inhibiting coating of single track can be realized and improve corrosion potential 100mV, reduces by 1 order of magnitude of corrosion electric current density.It present invention can be suitably applied to field of civil engineering.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene-based steel corrosion-inhibiting coating.
Background technique
Now and in later development time, structure of steel product is as knot important in building structure and field of civil engineering
Configuration formula has extremely important effect, while its corrosion resistance is also to determine the key of its service life.Over closer year, I
State's bridge spanning the sea, marine steel construction, coastal infrastructure are largely built up, ships used for military purposes, naval vessels steel demand obviously increase
Greatly, while because corrosion of steel is scrapped the steel quantity not being available increases, and huge national economy is caused to lose.Positioned at coastal
Steel and reinforced concrete structure in environment, the corrosion factors such as chloride ion, hydrone, oxygen molecule are contacted with steel substrate surface
It is the main reason for causing its burn into reduce its durability.In the spontaneous corrosion factor, such as the work of oxygen and water grading factors
Under, steel corrode.So the research of steel anti-corrosive durability is always state under coastal high salinity sea water intrusion environmental activity
Inside and outside hot spot.But previous anticorrosive paint using effect on high salinity seawater structure of steel product is not fine, and due to big
It requires to construct in the case where steel structure surface is dry, therefore is not particularly suited for built structure of steel product corrosion-inhibiting coating site operation.
Summary of the invention
The purpose of the present invention is to solve anticorrosion of steel structure coating antiseptic less effectives under high salinity briny environment to ask
Topic, provides a kind of preparation method of graphene-based steel corrosion-inhibiting coating.
A kind of preparation method of graphene-based steel corrosion-inhibiting coating of the present invention sequentially includes the following steps:
Step 1: steel surface is first subjected to degreasing and rust removal processing, is then polishing to light with polishing machine；
Step 2: the underwater curing epoxy resin that a layer thickness is 10 μm~30 μm is coated in the steel surface polished and is applied
Layer, then to its coagulation forming；
Step 3: silane coupling agent is diluted with distilled water, and volumetric concentration is 10~20% after dilution, dilution time
For 10-20min, it is then placed in spare in 25~50 DEG C of thermostat water baths；
Step 4: watersoluble plumbago alkene solution is spare with ultrasonic disperse 15min~30min；
Step 5: scattered watersoluble plumbago alkene in the silane coupling agent after diluting in step 3 and step 4 is pressed into volume
Ratio mixing than 1:1, it is spare to obtain black even mixed solution after stirring；
Step 6: steel obtained by step 2 are put into the mixed solution of step 5, are taken out, are put after impregnating 15~30min
It is spare to enter to dry 2h~4h in 80~100 DEG C of drying box；
Step 7: brushing a layer thickness is 10 μm~20 μm uniform oiliness graphenes again on the coating obtained by step 6, so
After be put into 80~100 DEG C of drying boxes dry 2h~4h after, that is, complete the coating of graphene-based steel corrosion-inhibiting coating.
The present invention is mixed to get evenly dispersed mixture using Kh550 silane coupling agent and watersoluble plumbago alkene, formed with
The transition zone that underwater curing epoxy resin is combined closely；Have the oiliness graphene of dissimilar polarities as face using with briny environment
Layer reduces surrounding medium sprawling in coating surface；Watersoluble plumbago alkene and oiliness graphite ene coatings collective effect, enhance coating
The effect of blocking to corrosive medium, and by increasing underwater curing epoxy resin/silane coupling agent watersoluble plumbago ene coatings
Coating road number, moreover it is possible to further promoted graphene corrosion-inhibiting coating anti-corrosion effect
The present invention has the advantage that steel surface is carried out degreasing and rust removal and grinding process by the present invention, water is then first used
Lower cured epoxy resin coats one layer of epoxy coating in the steel surface polished, then even using silane coupling agent, silane
Join agent watersoluble plumbago alkene composite layer, oiliness graphene layer Transition Technology, obtains to answer under littoral area, splash zone and high humidity environment
With and the excellent corrosion-inhibiting coating of antiseptic property, therefore can site operation for structure of steel product is completed.
It is not good enough in steel surface attachment that the graphene-based coating processes that the present invention is described can solve graphene-based coating
The problem of, it solves the problems, such as that graphene directly only forms Van der Waals force in steel substrate mating surface and Hydrogen bonding forces are poor, makes
The reliable covalent bond of formation and chemical bond, increase its stable bond power with steel substrate.It, can simultaneously compared with traditional handicraft
To solve the problems, such as the surface moisture in oceanic tide region steel construction matrix due to caused by the fluctuation tide of water, using underwater solid
Its environmental surfaces stable curing under water can be made by changing epoxy resin, while can also play chloride ion under exclusion of water, oxygen in air
Gas molecule, hydrone etc. accelerate the factor of steel substrate corrosion to reach substrate surface, play certain protective role.It mixes currently on the market
Adding anticorrosive paint of graphene etc. mostly is to be arrived using the dispersibility and barrier property of graphene sheet layer to increase corrosion medium factor
Up to the path of substrate surface, and there is no utilization, three layers of compound mistakes proposed by the invention for the barrier property of graphene lamella itself
The graphene-based coating processes for crossing coating can make graphene sheet layer be covered on bloom substrate surface, utilize the insulating of itself
Corrosion medium factor is isolated, steel antiseptic property can be made to greatly increase, the graphene-based steel corrosion-inhibiting coating of single track can be realized
The effect for improving corrosion potential 100mV, reducing by 1 order of magnitude of corrosion electric current density.It is apparent that the graphene-based steel of multiple tracks
Corrosion-inhibiting coating can further significantly improve anti-corrosion effect.
The present invention is obviously improved steel antiseptic property, and for the engineerings such as coastal, Oversea bridge, tunnel no matter
It is built or newly-built structure, can constructs under high humidity environment, the corrosion-inhibiting coating being had excellent performance.
Detailed description of the invention
Fig. 1 is graphene-based steel corrosion-inhibiting coating；
Fig. 2 is no anticorrosive coated steel test specimen salt spray test 10h steel surface of test piece pattern；
Fig. 3 is the steel test specimen salt spray test 10h steel surface of test piece pattern of comparative test 1；
Fig. 4 is the steel test specimen salt spray test 10h steel surface of test piece pattern for testing 1；
Fig. 5 is the scanning electron microscope pattern for testing the graphene-based steel corrosion-inhibiting coating of single track of 1 preparation；
Fig. 6 is the scanning electron microscope pattern of three graphene-based steel corrosion-inhibiting coatings of comparative test 2；
Fig. 7 has the Tafel polarization of graphene-based steel anticorrosive coated steel test specimen bent for no anticorrosive coated steel test specimen and test 1
Line；Wherein a is no anticorrosive coated steel test specimen, and b is that test 1 has graphene-based steel anticorrosive coated steel test specimen；
Fig. 8 is that test 1 has graphene-based steel corrosion-inhibiting coating to delineate test effect.
Specific embodiment
Specific embodiment 1: a kind of preparation method of graphene-based steel corrosion-inhibiting coating of present embodiment is according to the following steps
It carries out:
Step 1: steel surface is first subjected to degreasing and rust removal processing, is then polishing to light with polishing machine；
Step 2: the underwater curing epoxy resin that a layer thickness is 10 μm~30 μm is coated in the steel surface polished and is applied
Layer, then to its coagulation forming；
Step 3: silane coupling agent is diluted with distilled water, and volumetric concentration is 10~20% after dilution, dilution time
For 10-20min, it is then placed in spare in 25~50 DEG C of thermostat water baths；
Step 4: watersoluble plumbago alkene solution is spare with ultrasonic disperse 15min~30min；
Step 5: scattered watersoluble plumbago alkene in the silane coupling agent after diluting in step 3 and step 4 is pressed into volume
Ratio mixing than 1:1, it is spare to obtain black even mixed solution after stirring；
Step 6: steel obtained by step 2 are put into the mixed solution of step 5, are taken out, are put after impregnating 15~30min
It is spare to enter to dry 2h~4h in 80~100 DEG C of drying box；
Step 7: brushing a layer thickness is 10 μm~20 μm uniform oiliness graphenes again on the coating obtained by step 6, so
After be put into 80~100 DEG C of drying boxes dry 2h~4h after, that is, complete the coating of graphene-based steel corrosion-inhibiting coating.
Present embodiment has the advantages that steel surface is carried out degreasing and rust removal and grinding process by present embodiment, so
One layer of epoxy coating first is coated in the steel surface polished with underwater curing epoxy resin afterwards, then using silane coupled
Agent, silane coupling agent watersoluble plumbago alkene composite layer, oiliness graphene layer Transition Technology, obtaining can be in littoral area, splash zone and height
It is applied under wet environment and corrosion-inhibiting coating that antiseptic property is excellent.
The graphene-based coating processes that present embodiment is described can solve graphene-based coating and adhere in steel surface
Not good enough problem, solve graphene directly steel substrate mating surface only form Van der Waals force and Hydrogen bonding forces difference ask
Topic, is allowed to form reliable covalent bond and chemical bond, increases its stable bond power with steel substrate.Simultaneously with traditional handicraft phase
Than can solve the surface moisture problem in oceanic tide region steel construction matrix due to caused by the fluctuation tide of water, using
Underwater curing epoxy resin can make its environmental surfaces stable curing under water, while can also play chloride ion under exclusion of water, sky
Oxygen molecule, hydrone etc. accelerate the factor of steel substrate corrosion to reach substrate surface in gas, play certain protective role.City at present
It is to increase corrosive medium using the dispersibility and barrier property of graphene sheet layer that it is mostly that anticorrosive paint of graphene etc. is added on field
The factor reaches the path of substrate surface, and the barrier property of graphene lamella itself does not utilize, and proposed by the invention three layers
The graphene-based coating processes of compound tie coat can make graphene sheet layer be covered on bloom substrate surface, using itself
Corrosion medium factor is isolated in insulating, so that the steel antiseptic property is greatly increased the graphene-based steel corrosion-inhibiting coating of single track
Realize the effect for improving corrosion potential 100mV, reducing by 1 order of magnitude of corrosion electric current density.It is apparent that multiple tracks is graphene-based
Steel corrosion-inhibiting coating can further significantly improve anti-corrosion effect.
Present embodiment is obviously improved steel antiseptic property, and for the engineerings such as coastal, Oversea bridge, tunnel,
It is either completed still newly-built structure, can be constructed under high humidity environment, the corrosion-inhibiting coating being had excellent performance.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: underwater curing epoxy resin by
Component A and 100:(20~35 in mass ratio component B) ratio prepare, wherein component A is epoxy resin, and B component is underwater solid
Agent.Other are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: underwater curing asphalt mixtures modified by epoxy resin
Rouge is prepared by the ratio of component A and component B 100:21 in mass ratio.Other are the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: component A is bis-phenol
F epoxy resin, bisphenol A epoxide resin, novolac epoxy resin or o-cresol epoxy resin.Other and specific embodiment one to three
One of it is identical.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: B component is polyamides
Amine curing agent, fatty amines curing agent or phenolic aldehyde amine curing agent.Other are identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: steel surface removes
The method of oily processing of rust removing are as follows: using absorbent cotton dipping analysis absolute alcohol, wiping steel surface is until without floating iron mold mark；Then it uses
Deionized water carries out ultrasonic cleaning 10min to steel.Other are identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: silane coupling agent
For Kh550 silane coupling agent.Other are identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: step 4 be
Ultrasonic disperse is carried out under conditions of 150-200W, 40kHz.Other are identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: step 6 and step
Drying in rapid seven is drying 2h~4h in 80~100 DEG C of drying box.One of other and specific embodiment one to eight phase
Together.
Beneficial effects of the present invention are verified using following embodiment:
Test 1: a kind of preparation method of graphene-based steel corrosion-inhibiting coating of the present embodiment sequentially includes the following steps:
Step 1: processing 3c × 2 × 2cm3Steel test specimen, surface of test piece carry out degreasing and rust removal processing, then use polishing machine
Polishing surface-brightening, exposes the fresh surface of steel；
Step 2: the epoxy coating that a layer thickness is 15 μm is coated in surface of test piece, then to its coagulation forming；
Step 3: Kh550 silane coupling agent is diluted with distilled water, and the volumetric concentration after dilution is 20%, then
It is put into spare in 25 DEG C of thermostat water baths；
Step 4: by watersoluble plumbago alkene solution with spare after the ultrasonic disperse 15min of 180W, 40kHz, wherein watersoluble plumbago
Alkene solution is purchased from Nanjing Xian Feng Nono-material Science & Technology Ltd. commercial prod；
Step 5: by volume by Kh550 silane coupling agent obtained by step 3 and the scattered watersoluble plumbago alkene of step 4
It is spare to obtain black even mixed solution for the mixing of 1:1 after stirring；
Step 6: test specimen obtained by step 2 is put into the mixed solution of step 5, is taken out after impregnating 25min, is put into 80
Drying box drying 2h is spare at DEG C；.
Step 7: it is 15 μm of uniform oiliness graphenes by surface of test piece brushing a layer thickness obtained by step 6, is put into 80 DEG C
2h is dried in lower drying box, so final that arrive graphene-based steel corrosion-inhibiting coating as shown in Figure 1, medium oil graphene is purchased from south
Jing Xianfeng Nono-material Science & Technology Ltd. commercial prod.
Using embodiment one of the present invention, underwater curing epoxy as shown in Figure 1 is prepared in steel surface of test piece
Resin/silane coupling agent and watersoluble plumbago alkene it is compound/the graphene-based corrosion-inhibiting coating of three layers of oiliness graphene.By Fig. 1 it can be seen that,
The method of the invention can obtain fine and close graphene-based corrosion-inhibiting coating in steel surface.
In order to compare the effect of corrosion-inhibiting coating, this test is provided with comparative test:
Comparative test 1 is to sequentially include the following steps:
Step 1: processing 3c × 2 × 2cm3Steel test specimen, surface of test piece carry out degreasing and rust removal processing, then use polishing machine
Polishing surface-brightening, exposes the fresh surface of steel；
Step 2: the epoxy coating that a layer thickness is 15 μm is coated in surface of test piece, then to its coagulation forming；
Step 3: Kh550 silane coupling agent is diluted with distilled water, and the volumetric concentration after dilution is 20%, then
It is put into spare in 25 DEG C of thermostat water baths；
Step 4: by watersoluble plumbago alkene solution with spare after the ultrasonic disperse 15min of 180W, 40kHz, wherein watersoluble plumbago
Alkene solution is purchased from Nanjing Xian Feng Nono-material Science & Technology Ltd. commercial prod；
Step 5: by volume by Kh550 silane coupling agent obtained by step 3 and the scattered watersoluble plumbago alkene of step 4
It is spare to obtain black even mixed solution for the mixing of 1:1 after stirring；
Step 6: test specimen obtained by step 2 is put into the mixed solution of step 5, is taken out after impregnating 25min, is put into 80
Drying box dries 2h at DEG C, obtains the test specimen of applied in two coats watersoluble plumbago ene coatings.
Comparative test 2 is to sequentially include the following steps:
Step 1: processing 3c × 2 × 2cm3Steel test specimen, surface of test piece carry out degreasing and rust removal processing, then use polishing machine
Polishing surface-brightening, exposes the fresh surface of steel；
Step 2: the epoxy coating that a layer thickness is 15 μm is coated in surface of test piece, then to its coagulation forming；
Step 3: Kh550 silane coupling agent is diluted with distilled water, and the volumetric concentration after dilution is 20%, then
It is put into spare in 25 DEG C of thermostat water baths；
Step 4: by watersoluble plumbago alkene solution with spare after the ultrasonic disperse 15min of 150-200W, 40kHz, wherein aqueous
Graphene solution is purchased from Nanjing Xian Feng Nono-material Science & Technology Ltd. commercial prod；
Step 5: by volume by Kh550 silane coupling agent obtained by step 3 and the scattered watersoluble plumbago alkene of step 4
It is spare to obtain black even mixed solution for the mixing of 1:1 after stirring；
Step 6: test specimen obtained by step 2 is put into the mixed solution of step 5, is taken out after impregnating 25min, is put into 80
Drying box drying 2h is spare at DEG C；.
Step 7: it is 15 μm of uniform oiliness graphenes by surface of test piece brushing a layer thickness obtained by step 6, is put into 80 DEG C
2h is dried in lower drying box；
Step 8: being repeated twice the operation of step 2~step 7, obtains being coated with three graphene-based steel anti-corrosions paintings
The test specimen of layer.
Underwater curing epoxy resin in test 1 and comparative test 1,2 is by component A's and component B 100:21 in mass ratio
Ratio is prepared, and wherein component A is bisphenol A epoxide resin, B component is fatty amines curing agent.
Test 1, comparative test 1 and comparative test 2 are tested by GBT10125-2012 salt spray test standard, schemed
2-4 gives the surface topography that 10h salt fog acts on lower three kinds of steel test specimens.No anticorrosive coated steel test specimen shown in Fig. 2, due to salt fog
Corrosion electrochemistry effect lead to that more serious corrosion has occurred.Water of the test specimen of comparative test 1 shown in Fig. 3 due to salt fog
Solution effect, leads to coating global failure.It is shown in Fig. 4 using test 1 preparation underwater curing epoxy resin/silane coupling agent with
Watersoluble plumbago alkene is compound/the steel test specimen of the graphene-based corrosion-inhibiting coating of three layers of oiliness graphene, coating surface globality is good and nothing
Any local damage has excellent antiseptic property.
In order to further examine the surface state of graphene corrosion-inhibiting coating, using electron scanning Electronic Speculum for 1 preparation of test
The graphene-based steel corrosion-inhibiting coating of single track and three graphene-based steel corrosion-inhibiting coating surfaces of comparative test 2 seen
It surveys, as a result as illustrated in Figures 5 and 6.By Figures 5 and 6 it is found that the graphene corrosion-inhibiting coating prepared using single track and three techniques, is applied
Layer surface illustrates that corrosion-inhibiting coating has been achieved with smooth, close overlap joint without apparent buckling phenomena, can effectively prevent to corrode particle
Entrance.
Using the method for dynamic potential scanning, the test comparison corrosion protection effect of graphene corrosion-inhibiting coating, as a result such as Fig. 6
It is shown.It will be appreciated from fig. 6 that raising corrosion potential can be realized in the graphene-based steel corrosion-inhibiting coating of single track of 1 preparation of test
100mV, the effect for reducing by 1 order of magnitude of corrosion electric current density.
In order to investigate the performance of graphene corrosion-inhibiting coating more fully hereinafter, to the graphene-based steel of single track of the preparation of test 1
Corrosion-inhibiting coating carries out delineation test, as a result as shown in Figure 7.Compare ASTM D3359 coating adhesion standard, it is known that graphene is anti-
Rotten coating reaches 5B grades highest to the adhesive force of steel.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene-based steel corrosion-inhibiting coating, it is characterised in that this method sequentially includes the following steps:
Step 1: steel surface is first subjected to degreasing and rust removal processing, is then polishing to light with polishing machine；
Step 2: coating the underwater curing epoxy coating that a layer thickness is 10 μm~30 μm in the steel surface polished,
Then to its coagulation forming；
Step 3: silane coupling agent is diluted with distilled water, and volumetric concentration is 10~20% after dilution, and dilution time is
10-20min is then placed in spare in 25~50 DEG C of thermostat water baths；
Step 4: watersoluble plumbago alkene solution is spare with ultrasonic disperse 15min~30min；
Step 5: by scattered watersoluble plumbago alkene by volume 1 in the silane coupling agent after being diluted in step 3 and step 4:
1 ratio mixing, it is spare to obtain black even mixed solution after stirring；
Step 6: steel obtained by step 2 are put into the mixed solution of step 5, are taken out after impregnating 15~30min, are put into 80
It is spare that 2h~4h is dried in~100 DEG C of drying box；
Step 7: brushing a layer thickness is 10 μm~20 μm uniform oiliness graphenes again on the coating obtained by step 6, is then put
Enter after drying 2h~4h in 80~100 DEG C of drying boxes, that is, completes the coating of graphene-based steel corrosion-inhibiting coating.
2. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that underwater solid
Change epoxy resin by component A and 100:(20~35 in mass ratio component B) ratio prepare, wherein component A be epoxy resin, B
Group is divided into underwater curing agent.
3. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that underwater solid
Change epoxy resin to be prepared by the ratio of component A and component B 100:21 in mass ratio.
4. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 2 or 3, it is characterised in that A group
It is divided into bisphenol F epoxy resin, bisphenol A epoxide resin, novolac epoxy resin or o-cresol epoxy resin.
5. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 2 or 3, it is characterised in that B group
It is divided into polyamide-based curing agent, fatty amines curing agent or phenolic aldehyde amine curing agent.
6. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that steel table
The method of face degreasing and rust removal processing are as follows: using absorbent cotton dipping analysis absolute alcohol, wiping steel surface is until without floating iron mold mark；So
Ultrasonic cleaning 10min is carried out to steel with deionized water afterwards.
7. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that silane is even
Connection agent is Kh550 silane coupling agent.
8. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that step 4
It is that ultrasonic disperse is carried out under conditions of 150-200W, 40kHz.
9. a kind of preparation method of graphene-based steel corrosion-inhibiting coating according to claim 1, it is characterised in that step 6
It is drying 2h~4h in 80~100 DEG C of drying box with the drying in step 7.
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| CN116855152A (en) * | 2023-07-14 | 2023-10-10 | 长三角(海盐)纳米镀膜技术与智能装备研究院 | High-temperature wear-resistant coating applied to dental plate die and preparation method thereof |
| CN116855152B (en) * | 2023-07-14 | 2024-02-13 | 长三角(海盐)纳米镀膜技术与智能装备研究院 | High-temperature wear-resistant coating applied to dental plate die and preparation method thereof |
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