CN106987164B - A kind of preparation method of boron nitride-graphene oxide composite anti-corrosive filler - Google Patents
A kind of preparation method of boron nitride-graphene oxide composite anti-corrosive filler Download PDFInfo
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- CN106987164B CN106987164B CN201710349844.0A CN201710349844A CN106987164B CN 106987164 B CN106987164 B CN 106987164B CN 201710349844 A CN201710349844 A CN 201710349844A CN 106987164 B CN106987164 B CN 106987164B
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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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- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- 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
Abstract
The present invention provides a kind of boron nitride-graphene oxide composite anti-corrosive filler preparation methods, specially during preparing graphene oxide using improved Hummers method, boron nitride powder is added, while synthesizing graphene oxide, it can be achieved that graphene oxide and boron nitride it is compound.Present invention improves the hydrophily of graphene oxide and boron nitride, solve its bad dispersibility in organic resin, and its low problem of antiseptic property in epoxy coating.The synthetic method is easy to operate, it is easy to accomplish, cost is relatively low.The boron nitride of synthesis-graphene oxide compounded mix is added in epoxy resin to the corrosion resisting property that can increase substantially epoxy coating, the modification suitable for boron nitride and graphene oxide corrosion-inhibiting coating.
Description
Technical field
The present invention relates to anticorrosive paint fields, more particularly to a kind of boron nitride-graphene oxide composite anti-corrosive filler
Preparation method and application.
Background technique
Grapheme material is due to its unique lamellar structure, and good mechanical strength, high temperature resistant, chemical reactivity is low, makes
It causes extensive concern in anticorrosive paint field.But graphene compatibility in organic resin is poor, it is difficult to it is evenly dispersed,
And since its reactivity is low, it is difficult to realize effective modified.Graphene oxide equally has lamellar structure, not with graphene
Together, there is oxygen-containing functional group abundant on surface, and reactivity is high, this is advantageously implemented surface-functionalized modification.Boron nitride has
The features such as structure of class graphene, mechanical strength with higher, high temperature resistant, permeability resistance is strong, poorly conductive, these features
Make it suitable for applying in anticorrosive paint field.But the water imbibition of boron nitride and its compatibility poor with resin, which limit it, to be made
With.
At this stage for boron nitride and graphene complex method generally by high-temperature heat treatment, chemical vapor deposition etc.
Method, but these methods are there are complicated for operation, it is at high cost, be not suitable for the problem of producing in enormous quantities, be difficult to realize it in anti-corrosion
It is widely applied in coating.Research shows that there are mainly two types of the complex methods of boron nitride and graphene oxide: Publication No.
Method first ultrasonic in organic solution by boron nitride obtains lamella boron nitride in the Chinese patent of CN103480329A, then will
Graphene oxide made from Hummers method and lamella boron nitride obtained are ultrasonic in another organic solution, pass through ultrasound
Effect realize the compound of boron nitride and graphene oxide；The Chinese patent of Publication No. CN105349114A is used boron nitride
With the method for graphene oxide mixed processing in the specific dispersants such as neopelex, it is compound to obtain doping boron nitride
Material.The operating process of both methods is all more many and diverse, is unfavorable for realizing the extensive use in anticorrosive paint.
Summary of the invention
For graphene oxide and boron nitride, hydrophily is strong in the coating, bad dispersibility, the low problem of anti-corrosion ability, this hair
Bright purpose is to propose a kind of simple process, low in cost, and boron nitride and the graphene oxide suitable for batch production are compound
The preparation method of anticorrosive packing is, it can be achieved that it is used on a large scale in anticorrosive paint.
The present invention while synthesizing graphene oxide, realizes boron nitride and oxidation stone using improved Hummers method
Black alkene it is compound, reduce the hydrophily of graphene oxide and boron nitride, it is compound to effectively improve boron nitride-graphene oxide
Dispersibility and compatibility of the object in organic resin coating make the corrosion resistance of coating to improve the compactness of coating
It increases substantially.
The method of the present invention includes the following steps:
(1) graphite is mixed with boron nitride by certain mass ratio, addition sulfuric acid and phosphoric acid mixed liquor, under stirring slowly
Potassium permanganate is added, certain time is reacted under water-bath, removes excessive potassium permanganate with hydrogen peroxide after reaction.
(2) synthetic product is cleaned with the mode that a large amount of hydrochloric acid, ethyl alcohol and distilled water are centrifuged respectively, finally, freezing is dry
It is dry.
The mass ratio of the graphene and boron nitride is (0.01 ~ 0.99): (0.01 ~ 0.99).
The quality of the sulfuric acid and phosphoric acid mixed liquor is (100 ~ 200) times of graphite quality.
The volume ratio of sulfuric acid and phosphoric acid is (7 ~ 9) in the sulfuric acid and phosphoric acid mixed liquor: 1.
The quality of the potassium permanganate is (6 ~ 10) times of graphite quality.
The temperature of the water-bath is 45 ~ 70 DEG C.
The reaction time be 10 ~ for 24 hours.
The present invention is compound by boron nitride and graphene oxide, reduces the hydrophily of graphene oxide and boron nitride,
Dispersibility and compatibility of the boron nitride-graphene oxide compound in organic resin coating are effectively improved, painting is improved
The compactness of layer, hinders the diffusion of corrosive media in the coating, so as to improve the protective performance of coating.It is adopted in the present invention
Material and reagent price are cheap, the simple process of synthesis, easy to implement, at low cost.The present invention is by boron nitride and aoxidizes stone
Black alkene is compound, not only increases substantially the corrosion resistance of coating, and for subsequent other pigments and fillers it is compound provide it is good
Good basis is of great significance to the engineering application for promoting organic anti-corrosive coating.
Detailed description of the invention
Fig. 1 is graphene oxide, boron nitride and boron nitride-graphene oxide compound infrared spectrogram.
Fig. 2 is N1s element spectrogram in boron nitride (a) and boron nitride-graphene oxide compound (b) photoelectron spectroscopy.
Fig. 3 is that graphene oxide (a), boron nitride (b) and boron nitride-graphene oxide compound (c) transmission electron microscope shine
Piece.
Fig. 4 is graphene oxide (a), boron nitride (b) and boron nitride-graphene oxide compound (c) contact angle photo.
Fig. 5 be graphite oxide ene coatings (a), boron nitride coating (b), boron nitride-graphene oxide mixed coating (c) and
Boron nitride-graphene oxide composite coating (d) stereoscan photograph.
Fig. 6 is graphite oxide ene coatings, boron nitride coating, boron nitride-graphene oxide mixed coating and nitridation boron-oxygen
Graphite alkene composite coating impregnates the modulus value figure in 1160 hours electrochemical impedance spectroscopy Bode figures in 3.5%NaCl solution.
Fig. 7 is graphite oxide ene coatings, boron nitride coating, boron nitride-graphene oxide mixed coating and nitridation boron-oxygen
Graphite alkene composite coating impregnates the Nyquist figure of 1160 hours electrochemical impedance spectrograms in 3.5%NaCl solution.
Specific embodiment
The present invention will be described in detail with reference to the accompanying drawing and by specific embodiment and comparative example, so that of the invention
Advantages and features can be easier to be readily appreciated by one skilled in the art, to make to protection scope of the present invention apparent clear
Define.
Comparative example 1: the preparation of graphite oxide ene coatings
(1) graphene oxide reaction process: 3g graphite is put into the flask of 500mL, and the 270mL concentrated sulfuric acid and 30mL is added
The mixed acid of phosphoric acid is uniformly mixed under the action of magnetic agitation.The potassium permanganate for claiming 18g, is added slowly to above-mentioned solution
In, 15h is reacted under 50 DEG C of water-baths, magnetic agitation continues entire synthesis process, is down to room temperature after reaction.Reaction solution is fallen
Enter in the ice water of 500mL, 30% hydrogen peroxide is added dropwise while magnetic agitation, until solution colour becomes glassy yellow.
(2) graphene oxide is cleaned and dried process: the solution after reaction being centrifuged, the salt of the product 400mL after centrifugation
Acid centrifuging cleans twice, to pH is wash with distilled water finally 6 ~ 7 then with twice of ethyl alcohol eccentric cleaning.By the oxidation stone of acquisition
Black alkene is put into freeze dryer dry for 24 hours to get to graphene oxide filler.
(3) preparation of graphite oxide ene coatings: by graphene oxide filler, epoxy resin, dimethylbenzene and n-butanol in ball
It is mixed in grinding jar, mill pearl is added.After being dispersed with ball mill, lapping liquid is poured out into weighing, curing agent polyamide is added.It stirs evenly
It is applied on the metallic matrix pre-processed afterwards, solidification is stand-by.
Comparative example 2: the preparation of boron nitride coating:
The boron nitride filler of purchase, epoxy resin, dimethylbenzene and n-butanol are mixed in ball grinder, mill pearl is added.With
After ball mill dispersion, lapping liquid is poured out into weighing, curing agent polyamide is added.It is applied to the metal pre-processed after mixing evenly
On matrix, solidification is stand-by.
Comparative example 3: boron nitride-graphene oxide mixed coating preparation
Step (1) and (2) are identical as comparative example 1；
(3) boron nitride-graphene oxide mixed coating preparation: the boron nitride of purchase and graphene oxide obtained are mixed
It closes, then is mixed in ball grinder with epoxy resin, dimethylbenzene and n-butanol, mill pearl is added.After being dispersed with ball mill, by lapping liquid
Weighing is poured out, curing agent polyamide is added.It is applied on the metallic matrix pre-processed after mixing evenly, solidification is stand-by.
Embodiment 1: boron nitride-graphene oxide composite coating preparation
(1) boron nitride-graphene oxide reaction process: 3g graphite and 3g hexagonal boron nitride are put into the flask of 500mL,
The mixed acid of the 270mL concentrated sulfuric acid and 30mL phosphoric acid is added, is uniformly mixed under the action of magnetic agitation.Weigh the permanganic acid of 18g
Potassium is added slowly in above-mentioned solution, and 15h is reacted under 50 DEG C of water-baths, and magnetic agitation continues entire synthesis process, reaction knot
Room temperature is down to after beam.Reaction solution is poured into the ice water of 500mL, 30% hydrogen peroxide is added dropwise while magnetic agitation, until
Solution colour becomes glassy yellow.
(2) boron nitride-graphene oxide is cleaned and dried process: the solution after reaction being centrifuged, the product after centrifugation is used
Twice of the hydrochloric acid eccentric cleaning of 400mL, then with twice of ethyl alcohol eccentric cleaning to pH is wash with distilled water finally 6 ~ 7.It will obtain
Boron nitride-graphene oxide compound be put into freeze dryer it is dry for 24 hours to get to boron nitride-graphene oxide composite anti-corrosive
Filler.
(3) boron nitride-graphene oxide composite coating preparation: by boron nitride-graphene oxide compounded mix, asphalt mixtures modified by epoxy resin
Rouge, dimethylbenzene and n-butanol mix in ball grinder, and mill pearl is added.After being dispersed with ball mill, lapping liquid is poured out into weighing, is added
Curing agent polyamide.It is applied on the metallic matrix pre-processed after mixing evenly, solidification is stand-by.
Embodiment 2: boron nitride-graphene oxide composite coating preparation
(1) boron nitride-graphene oxide reaction process: 3g graphite and 1g hexagonal boron nitride are put into the flask of 500mL,
The mixed acid of the 540mL concentrated sulfuric acid and 60mL phosphoric acid is added, is uniformly mixed under the action of magnetic agitation.Claim the potassium permanganate of 30g,
It is added slowly in above-mentioned solution, 18h is reacted under 50 DEG C of water-baths, magnetic agitation continues entire synthesis process, and reaction terminates
After be down to room temperature.Reaction solution is poured into the ice water of 500mL, 30% hydrogen peroxide, Zhi Daorong are added dropwise while magnetic agitation
Liquid color becomes glassy yellow.
(2) boron nitride-graphene oxide is cleaned and dried process: the solution after reaction being centrifuged, the product after centrifugation is used
Twice of the hydrochloric acid eccentric cleaning of 400mL, then with twice of ethyl alcohol eccentric cleaning to pH is wash with distilled water finally 6 ~ 7.It will obtain
Boron nitride-graphene oxide compound be put into freeze dryer it is dry for 24 hours to get to boron nitride-graphene oxide compounded mix.
(3) boron nitride-graphene oxide composite coating preparation: by boron nitride-graphene oxide compounded mix, asphalt mixtures modified by epoxy resin
Rouge, dimethylbenzene and n-butanol mix in ball grinder, and mill pearl is added.After being dispersed with ball mill, lapping liquid is poured out into weighing, is added
Curing agent polyamide.It is applied on the metallic matrix pre-processed after mixing evenly, solidification is stand-by.
Graphene oxide, boron nitride and boron nitride-graphene oxide compounded mix powder are directly carried out respectively infrared
Spectrum test obtains Fig. 1.BN represents boron nitride in figure, and GO represents graphene oxide, and BN-GO represents boron nitride-graphene oxide
Compounded mix.There is the feature of graphene oxide in boron nitride-graphene oxide compound infrared spectroscopy as we can see from the figure
Functional group, while characteristic group's absorption peak of boron nitride shifts, this illustrates nitrogen in boron nitride-graphene oxide compound
Change and is interacted in boron with graphene oxide.
Graphene oxide, boron nitride and boron nitride-graphene oxide compounded mix powder are subjected to XPS test respectively,
Obtain Fig. 2.The nitrogen in boron nitride-graphene oxide compound has also appeared N-in addition to there is B-N key as we can see from the figure
O key illustrates that the O element in N element and graphene oxide in boron nitride is chemically bonded.
Transmission electron microscope (TEM) observation is carried out to graphene oxide, boron nitride and boron nitride-graphene oxide compounded mix.
Graphene oxide is flaky texture in Fig. 3, and boron nitride is disc-shaped structure, in boron nitride-graphene oxide compounded mix
Boron nitride particle is scattered between the surface or lamellar structure of graphene oxide layer structure, this structure be conducive to boron nitride with
Graphene oxide collaboration improves antiseptic property.
After graphene oxide, boron nitride and boron nitride-graphene oxide compounded mix powder tabletting machine, into
Row contact angle test.As seen from Figure 4, contact angle of the boron nitride-between graphene oxide compound and distilled water is greater than single
The contact angle of the contact angle of pure boron nitride and simple graphene oxide, this illustrates to drop after boron nitride and graphene oxide are compound
Low hydrophily improves the compatibility with resin.
To graphite oxide ene coatings, boron nitride coating, boron nitride-graphene oxide mixed coating and boron nitride-oxidation stone
Black alkene composite coating is scanned Electronic Speculum (SEM) observation.From fig. 5, it is seen that graphite oxide ene coatings and boron nitride coating
In all there is serious reunion and boundary defect, graphene oxide is added in coating after mixing with boron nitride, agglomeration and
Boundary defect is more serious, and boron nitride-graphene oxide it is compound after be added in coating, agglomeration of the filler in resin
Alleviate, boundary defect reduces.Since boron nitride and the compound rear hydrophily of graphene oxide reduce, keep its dispersion in resin equal
Even property and interface compatibility improve.
Using electrochemical workstation to graphite oxide ene coatings, boron nitride coating, boron nitride-graphene oxide mixed coating
Electrochemical impedance spectroscopy test is carried out respectively with boron nitride-graphene oxide composite coating.BN represents boron nitride in figure, and GO represents oxygen
Graphite alkene.As seen from Figure 6, boron nitride-graphene oxide composite coating low-frequency impedance modulus value highest in Bode figure, figure
Capacitive reactance arc radius is maximum in 7 Nyquist figure, illustrates that boron nitride-graphene oxide composite coating makees the blocking of corrosive medium
With preferable, outstanding behaviours goes out excellent Corrosion Protection.
It in summary it can be seen, the present invention while synthesizing graphene oxide, can be realized using improved Hummers method
It is compound between boron nitride and graphene oxide, this compound can improve boron nitride and graphene oxide and epoxy resin it
Between interface compatibility, reduce epoxy coating in boundary defect, improve the protective performance of coating.
Claims (7)
1. a kind of boron nitride-graphene oxide composite anti-corrosive filler preparation method, it is characterised in that include the following steps:
(1) graphite is mixed with hexagonal boron nitride by certain mass ratio, addition sulfuric acid and phosphoric acid mixed liquor, under stirring slowly
Potassium permanganate is added, certain time is reacted under water-bath, removes excessive potassium permanganate with hydrogen peroxide after reaction；
(2) synthetic product is cleaned with the mode that a large amount of hydrochloric acid, ethyl alcohol and distilled water are centrifuged respectively, finally, freeze-drying.
2. preparation method according to claim 1, it is characterised in that the mass ratio of the graphite and hexagonal boron nitride is
(0.01~0.99): (0.01~0.99).
3. preparation method according to claim 1, it is characterised in that the sulfuric acid is (7~9) with phosphoric acid volume ratio: 1.
4. preparation method according to claim 1, it is characterised in that the quality of the sulfuric acid and phosphoric acid mixed liquor is graphite
(100~200) of quality times.
5. preparation method according to claim 1, it is characterised in that the quality of the potassium permanganate is (the 6 of graphite quality
~10) again.
6. preparation method according to claim 1, it is characterised in that the temperature of the water-bath is 45~70 DEG C.
7. preparation method according to claim 1, it is characterised in that the reaction time be 10~for 24 hours.
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| CN110204991B (en) * | 2019-04-28 | 2021-09-17 | 西南石油大学 | Efficient anticorrosion h-BN/GO/waterborne epoxy composite material, preparation method and application |
| CN111117313B (en) * | 2019-12-31 | 2021-02-19 | 浙江大学 | High-hardness normal-temperature-cured geopolymer metal anticorrosive paint and preparation method thereof |
| CN113637338B (en) * | 2021-08-18 | 2022-10-14 | 天津大学 | Modified hexagonal boron nitride, water-based anti-oxidation anticorrosive coating and preparation method thereof |
| CN116463028A (en) * | 2023-04-06 | 2023-07-21 | 郑州艾洁环保设备科技有限公司 | Preparation method of metal surface anti-corrosion coating |
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