CN110128916A - A kind of preparation method of graphene/epoxy flake anticorrosive paint - Google Patents
A kind of preparation method of graphene/epoxy flake anticorrosive paint Download PDFInfo
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- CN110128916A CN110128916A CN201910472163.2A CN201910472163A CN110128916A CN 110128916 A CN110128916 A CN 110128916A CN 201910472163 A CN201910472163 A CN 201910472163A CN 110128916 A CN110128916 A CN 110128916A
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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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- 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
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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)
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Abstract
The invention discloses a kind of graphene/epoxy flake anticorrosive paint preparation methods, using large stretch of graphene oxide water solution as raw material, reducing agent are added and is self-assembled into graphene microgel；Graphene microgel is modified using modifying agent；Modified graphene microgel, epoxy resin, curing agent and defoaming agent mixing after-pouring obtain graphene/epoxy scale anticorrosion coating of high antiseptic property.The present invention prepares graphene scale anticorrosion coating, the simple process, at low cost, suitable large-scale industrial production using graphene microgel-modifier modification-pouring molding method.
Description
Technical field
The invention belongs to flake anticorrosive paint preparation field more particularly to a kind of graphene/epoxy flake anticorrosive paints
Preparation method.
Background technique
Epoxy resin typically refers to the high molecular material in strand containing two or more epoxy groups, its master
Chain also has epoxy group and other oxygen-containing groups usually based on aromatic series, alicyclic or aliphatic segment on main chain
The high-molecular oligomers body formed reacts with curing agent (mainly including fatty amine, polyamide and anacardol etc.) by epoxy group in group.
As heat reactive resin, it is exhausted that epoxy resin has excellent adhesion energy, resistance to abrasion, mechanical property, chemical stability, electric appliance
Edge and shrinking percentage is low, easy processing molding, preferable stress transfer and it is low in cost the advantages that, in coating, machinery, space flight
The every field such as aviation, building are got a lot of applications, and are one of the basic resins being most widely used in polymer material.It is rotten
One of 3 kinds of principal modes as material failure are lost, great harm is caused to national economy, is increasingly ground both at home and abroad
Study carefully the concern of personnel.However, epoxy resin solidifies post-crosslinking density height as anticorrosive paint, it is in tridimensional network, hardness
Greatly, flexibility is insufficient, and due to containing benzene nucleus in molecular structure, resin cured matter weatherability is poor, especially intolerant to ultraviolet light.
Epoxy coating non-refractory, mechanical strength is lower at high temperature, at the same during film-forming micropore easy to form and
The compactness of epoxy coating is reduced, while with the continuous continuous complexity expanded with use environment of epoxy resin application range
Change, new requirement is had also been proposed to the antiseptic property of epoxy resin, therefore, it is necessary to epoxy coating carry out functional modification to
Improve its integrated protection performance.Currently, the main path for improving epoxy resin antiseptic property both at home and abroad includes epoxy molecule
Chemical modification and nano inorganic filler modified epoxy.Nano inorganic filler is modified have simple process, performance boost it is significant,
The advantages such as production cost is low become the main direction of studying that epoxy resin improves antiseptic property.
Graphene is by sp2A kind of new carbon with bi-dimensional cellular shape structure that carbon atom is constituted, it is unique
Monoatomic layer structure assigns its excellent physical and chemical performance, and graphene has brilliant mechanical property, excellent conductive and heat-conductive
Performance, the two-dimensional structure of graphene makes it have more preferably shielding and barrier property, while graphene can pass through reduction-oxidation
Graphene method realizes large-scale production, it is considered to be optimal composite coating nano modified filler.
The addition of graphene can effectively improve the antiseptic property of epoxy composite coating, but graphene is by hexa-atomic aromatic rings structure
At there are stronger Van der Waals forces for piece interlayer, are also easy to produce stacking, the graphene of heap poststack vapor channel easy to form causes to apply
The compactness of layer substantially reduces.Therefore, the reunion problem for solving graphene oxide, improve its in the epoxy dispersibility and
Compatibility, the graphene/epoxy scale anticorrosion coating for obtaining orderly laminated construction are imperative.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of preparations of graphene/epoxy flake anticorrosive paint
Method, selecting large stretch of graphene oxide (LGO) is raw material, and graphene microgel is self-assembled into the presence of reducing agent,
And add it in epoxy resin, casting method prepares graphene/epoxy scale anticorrosion coating, and graphene microgel is spontaneous heavy
Under force field, it is self-assembly of the composite coating of scale laminated construction, plays " the labyrinth effect " of scale laminated construction, is obtained
High performance graphene composite coating, coating salt-fog resistant time prepared by the present invention are greater than 1000 hours.
Preparation method of the present invention is realized especially by following technical scheme:
A kind of preparation method of graphene/epoxy flake anticorrosive paint, specifically includes the following steps:
1) using graphene oxide water solution as raw material, reducing agent is added, is reacted at 50 DEG C, graphene oxide partial reduction
Form microgel；
2) graphene microgel solution is stirred and heated to 50 DEG C, it is molten that modifying agent is slowly added into graphene microgel
It is reacted in liquid, after filtering, deionized water cleaning, freeze-drying；
3) the graphene microgel powder after freeze-drying is added in dimethylbenzene/butanol solution, concussion is dispersed into
Even solution, adds epoxy resin, curing agent and defoaming agent, and casting method prepares coating is self-assembly of scale anticorrosion coating.
Further, the concentration of graphene oxide solution described in step (1) is 2~10mg/mL, graphene oxide sheet
Layer is having a size of 100~500 μm.
Further, reducing agent described in step (1) is selected from hydroiodic acid, sodium borohydride, ascorbic acid or ascorbic acid
One of sodium kind.
Further, the mass ratio of reducing agent and graphene oxide is 2:1~5:1, reaction time 10- in step (1)
70min。
Further, it is even to be selected from dodecanamide propyl amine oxide, polyvinyl alcohol or silane for modifying agent described in step (2)
Join one of agent KH550 kind, the reaction time is 30~60min.
Further, curing agent described in step (3) is Versamid curing agent 650, and the defoaming agent is
Surfynol DF220, the dimethylbenzene/butanol solution are the mixing of dimethylbenzene/n-butanol mass ratio 5~9:1~4
Solution.
The invention has the benefit that
Selected modifying agent is environmentally protective, low in cost, and modified technique is simple, mild condition, effect are good, easy large-scale industry
Metaplasia produces；Modified graphene microgel is self-assembly of scale structure in the epoxy, plays the labyrinth of scale structure
Effect obtains the composite coating of excellent protective performance.
The present invention prepares graphene/epoxy scale using graphene microgel-modifier modification-pouring molding method and prevents
Rotten coating, the simple process, at low cost, suitable large-scale industrial production.
Modified graphene microgel is dispersed in epoxy resin solution, pours rear graphene microgel spontaneous
Scale structure is formed under the action of gravity, prepares the composite coating of high antiseptic property, meets auto industry, power industry, ship
Requirement of the fields such as oceangoing ship, marine industry, electronics industry, container industry to the antiseptic property of epoxy coating.
Detailed description of the invention
Fig. 1 is graphene of the present invention/epoxy flake anticorrosive paint preparation method flow chart.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is explained in detail with reference to the accompanying drawing.
As shown in Figure 1, a kind of preparation method of graphene/epoxy flake anticorrosive paint provided in an embodiment of the present invention includes
Following steps:
S101: using large stretch of graphene oxide water solution as raw material, being added reducing agent, react the regular hour at 50 DEG C,
Graphene oxide partial reduction forms microgel, and wherein the concentration of graphene oxide is 2~10mg/mL, graphene oxide layer
Having a size of 100~500 μm, reducing agent is one of hydroiodic acid, sodium borohydride, ascorbic acid, sodium ascorbate, reducing agent with
The mass ratio of graphene oxide is 2:1~5:1, reaction time 10-70min；
S102: graphene microgel solution movement is stirred and heated to 50 DEG C；It is micro- that modifying agent is slowly added into graphene
In gel solution, certain time is reacted, filtering, deionized water cleaning, freeze-drying, wherein modifying agent is dodecanamide propyl oxygen
Change one kind of amine, polyvinyl alcohol or Silane coupling agent KH550, the reaction time is 30~60min；
S103: the graphene microgel powder after freeze-drying is added in dimethylbenzene/butanol solution, concussion is dispersed into
Uniform solution adds epoxy resin, curing agent and defoaming agent, continues to stir 30min, vacuumizes degasification after standing 10min
Bubble, casting method prepares coating, graphene microgel are self-assembly of scale anticorrosion coating under spontaneous gravity field action.
The invention will be further described combined with specific embodiments below.
Embodiment 1
The concentration of large stretch of graphene oxide water solution is 3mg/L, and graphene oxide layer average-size is 100 μm, is added
The hydroiodic acid of 3 times of its quality reacts 30min at 50 DEG C, obtains graphene microgel.Graphene microgel solution movement stirs simultaneously
It is heated to 50 DEG C；Modifying agent dodecanamide propyl amine oxide is slowly added into graphene microgel solution, 60min is reacted,
Filtering, deionized water cleaning, freeze-drying；Modified graphene microgel powder 0.8g after freeze-drying is added to mass ratio
For in dimethylbenzene/butanol solution of 8:3, concussion is dispersed into uniform solution, then the epoxy resin of 25g is added to three mouthfuls of burnings
In bottle, lg curing agent and 0.25g defoaming agent is added, continues to stir 30min, vacuumizes bubble removing after standing 10min, pour legal system
Standby coating.
Above-mentioned resulting graphene/epoxy scale anticorrosion coating salt-fog resistant time is greater than 1100 hours.
Embodiment 2
The concentration of large stretch of graphene oxide water solution is 2mg/L, and graphene oxide layer average-size is 150 μm, is added
The sodium ascorbate of 2 times of its quality reacts 40min at 50 DEG C, obtains graphene microgel.Graphene microgel solution movement stirs
It mixes and is heated to 50 DEG C；Modifying agent polyvinyl alcohol is slowly added into graphene microgel solution, 50min is reacted, filters, goes
Ionized water cleaning, freeze-drying；Modified graphene microgel powder 1g after freeze-drying is added to two that mass ratio is 7:3
In toluene/butanol solution, concussion is dispersed into uniform solution, then the epoxy resin of 25g is added in three-necked flask, is added
Lg curing agent and 0.25g defoaming agent continue to stir 30min, vacuumize bubble removing, casting method prepares coating after standing 10min.
Above-mentioned resulting graphene/epoxy scale anticorrosion coating salt-fog resistant time is greater than 1200 hours.
Embodiment 3
The concentration of large stretch of graphene oxide water solution is 5mg/L, and graphene oxide layer average-size is 100 μm, is added
The sodium borohydride of 3 times of its quality reacts 30min at 50 DEG C, obtains graphene microgel.The stirring of graphene microgel solution movement
And it is heated to 50 DEG C；Modifying agent Silane coupling agent KH550 is slowly added into graphene microgel solution, 45min, mistake are reacted
Filter, deionized water cleaning, freeze-drying；Modified graphene microgel powder 0.6g after freeze-drying, which is added to mass ratio, is
In dimethylbenzene/butanol solution of 6:2, concussion is dispersed into uniform solution, then the epoxy resin of 25g is added to three-necked flask
In, lg curing agent and 0.25g defoaming agent is added, continues to stir 30min, vacuumizes bubble removing, casting method preparation after standing 10min
Coating.
Above-mentioned resulting graphene/epoxy scale anticorrosion coating salt-fog resistant time is greater than 1050 hours.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of graphene/epoxy flake anticorrosive paint preparation method, which comprises the following steps:
1) using large stretch of graphene oxide water solution as raw material, reducing agent is added, is reacted at 50 DEG C, graphene oxide partial reduction
Form microgel；
2) graphene microgel solution is stirred and heated to 50 DEG C, modifying agent is slowly added into graphene microgel solution
Reaction, after filtering, deionized water cleaning, freeze-drying；
3) the graphene microgel powder after freeze-drying is added in dimethylbenzene/butanol solution, concussion is dispersed into uniform
Solution, adds epoxy resin, curing agent and defoaming agent, and casting method prepares coating is self-assembly of scale anticorrosion coating.
2. preparation method according to claim 1, which is characterized in that graphene oxide solution described in step (1)
Concentration is 2~10mg/mL, and graphene oxide layer is having a size of 100~500 μm.
3. preparation method according to claim 1, which is characterized in that the reducing agent be selected from hydroiodic acid, sodium borohydride,
One of ascorbic acid or sodium ascorbate kind.
4. preparation method according to claim 1, which is characterized in that the matter of reducing agent and graphene oxide in step (1)
Amount is than being 2:1~5:1.
5. preparation method according to claim 1, which is characterized in that the modifying agent is aoxidized selected from dodecanamide propyl
One of amine, polyvinyl alcohol or Silane coupling agent KH550 kind.
6. preparation method according to claim 1, which is characterized in that the curing agent is polyamide curing agent 650.
7. preparation method according to claim 1, which is characterized in that the defoaming agent is Surfynol DF220.
8. preparation method according to claim 1, which is characterized in that the dimethylbenzene/butanol solution is mass ratio 5
The mixed solution of~9:1~4.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713773A (en) * | 2019-09-25 | 2020-01-21 | 界首市金龙机械设备有限公司 | Coating liquid for preventing paint surface from being defective after paint spraying |
| CN111019499A (en) * | 2019-11-02 | 2020-04-17 | 上海弘吉印刷科技有限公司 | Method for manufacturing thermal transfer printing coating material |
| CN113005016A (en) * | 2021-03-23 | 2021-06-22 | 江西省农业科学院农业应用微生物研究所（江西省农村能源研究中心） | Biochar-mediated two-phase anaerobic fermentation biogas production device for collecting culture feces in full-quantitative manner and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1116760A2 (en) * | 2000-01-11 | 2001-07-18 | Shin-Etsu Chemical Co., Ltd. | Coated articles |
| CN104085143A (en) * | 2014-05-29 | 2014-10-08 | 深圳市铭晶科技有限公司 | Preparation method of composite heat conduction graphene film and composite heat conduction graphene film |
| CN106675320A (en) * | 2016-11-22 | 2017-05-17 | 北京国电富通科技发展有限责任公司 | Graphene heat-conduction anticorrosion paint and preparation method thereof |
| CN108341929A (en) * | 2018-03-19 | 2018-07-31 | 温岭市创嘉信息科技有限公司 | A kind of Graphene epoxy resin composite material and preparation method thereof |
| CN109337505A (en) * | 2018-09-17 | 2019-02-15 | 成都新柯力化工科技有限公司 | A kind of corrosion-resistant graphene oxide/aqueous epoxide resin paint and preparation method |
| CN109627904A (en) * | 2018-11-07 | 2019-04-16 | 西北工业大学 | A kind of selfreparing graphene zinc-rich anti-corrosive paint and preparation method thereof |
-
2019
- 2019-05-31 CN CN201910472163.2A patent/CN110128916A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1116760A2 (en) * | 2000-01-11 | 2001-07-18 | Shin-Etsu Chemical Co., Ltd. | Coated articles |
| CN104085143A (en) * | 2014-05-29 | 2014-10-08 | 深圳市铭晶科技有限公司 | Preparation method of composite heat conduction graphene film and composite heat conduction graphene film |
| CN106675320A (en) * | 2016-11-22 | 2017-05-17 | 北京国电富通科技发展有限责任公司 | Graphene heat-conduction anticorrosion paint and preparation method thereof |
| CN108341929A (en) * | 2018-03-19 | 2018-07-31 | 温岭市创嘉信息科技有限公司 | A kind of Graphene epoxy resin composite material and preparation method thereof |
| CN109337505A (en) * | 2018-09-17 | 2019-02-15 | 成都新柯力化工科技有限公司 | A kind of corrosion-resistant graphene oxide/aqueous epoxide resin paint and preparation method |
| CN109627904A (en) * | 2018-11-07 | 2019-04-16 | 西北工业大学 | A kind of selfreparing graphene zinc-rich anti-corrosive paint and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110713773A (en) * | 2019-09-25 | 2020-01-21 | 界首市金龙机械设备有限公司 | Coating liquid for preventing paint surface from being defective after paint spraying |
| CN111019499A (en) * | 2019-11-02 | 2020-04-17 | 上海弘吉印刷科技有限公司 | Method for manufacturing thermal transfer printing coating material |
| CN113005016A (en) * | 2021-03-23 | 2021-06-22 | 江西省农业科学院农业应用微生物研究所（江西省农村能源研究中心） | Biochar-mediated two-phase anaerobic fermentation biogas production device for collecting culture feces in full-quantitative manner and application |
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