CN109111782A - The preparation method of modified graphene oxide dispersion liquid and modified electrophoretic coating - Google Patents
The preparation method of modified graphene oxide dispersion liquid and modified electrophoretic coating Download PDFInfo
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- CN109111782A CN109111782A CN201810798393.3A CN201810798393A CN109111782A CN 109111782 A CN109111782 A CN 109111782A CN 201810798393 A CN201810798393 A CN 201810798393A CN 109111782 A CN109111782 A CN 109111782A
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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
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
- C09D5/443—Polyepoxides
- C09D5/4457—Polyepoxides containing special additives, e.g. pigments, polymeric particles
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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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- 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
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
- C09D5/443—Polyepoxides
- C09D5/4453—Polyepoxides characterised by the nature of the curing agent
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Abstract
The present invention discloses the preparation method and electrophoretic coating of modified graphene oxide dispersion liquid, wherein, the preparation method of modified graphene oxide dispersion liquid, the following steps are included: α 1, taking the graphene oxide powder of 1 mass fraction, then the deionized water of 1250 mass fractions is added, 1h is stirred, the dispersion liquid of graphene oxide is made；α 2, the graphene oxide dispersion is heated to 80-90 DEG C, slowly instills the p-phenylenediamine of 5 mass fractions, slowly stirs, until powder all dissolves, then keep the temperature 2-3h, deep purple solution is made；α 3, the solution of the darkviolet is filtered, is then washed repeatedly with deionized water and dehydrated alcohol again, obtain modified graphene oxide aqueous dispersion.P-phenylenediamine be modified after graphene oxide, can preferably be dispersed in electrophoresis groove liquid, compatibility is more preferable.
Description
Technical field
The present invention relates to the technical field of electrophoretic coating, in particular to the preparation method of modified graphene oxide dispersion liquid and
Modified electrophoretic coating.
Background technique
The one kind of electrophoretic coating as water paint both has low VOC, environmentally protective, but also with high degree of automation, applies
Expect the high feature of utilization rate.95% or more is had reached in the use of automobile industry.With to the higher and higher of requirement for anticorrosion, coating
Developer needs constantly seeking new technology, to promote its antiseptic property.
Summary of the invention
The object of the present invention is to provide the preparation method of modified graphene oxide dispersion liquid and electrophoretic coatings, solve above-mentioned existing
There is one or more in technical problem.
The preparation method of modified graphene oxide dispersion liquid provided by the invention, comprising the following steps:
Then the deionized water of 1250 mass fractions is added in α 1, the graphene oxide powder for taking 1-5 mass fraction, stirring
The dispersion liquid of graphene oxide is made in 1h；
α 2, the graphene oxide dispersion is heated to 80-90 DEG C, slowly instills the p-phenylenediamine of 5-8 mass fraction,
It slowly stirs, until powder all dissolves, then keeps the temperature 2-3h, deep purple solution is made；
α 3, the solution of the darkviolet is filtered, is then washed, is obtained repeatedly with deionized water and dehydrated alcohol again
Modified graphene oxide aqueous dispersion.
A kind of modified electrophoretic coating, the modified graphene oxide dispersion liquid obtained including above-mentioned preparation method and main body cream
Liquid.
In some embodiments, main body lotion preparation method the following steps are included:
β 1, small molecule base epoxy resin, chain extender, catalyst, organic solvent are added in the reaction vessel, in 120-
Chain extending reaction is carried out between 160 DEG C, obtains the macromolecular epoxy resin that epoxide equivalent is 1000-3000；
β 2, epoxide equivalent be 1000-3000 macromolecular epoxy resin in, be stirred continuously down and be warming up to 90-95 DEG C, add
Enter the amine compounds containing active hydrogen, be warming up to 115-125 DEG C, then keep the temperature 3 hours, obtains the main body epoxy of amine modification after chain extension
Resin；
Main body epoxy resin, the Blocked Isocyanate Curing Agents that amine is modified after addition chain extension in β 3, reaction vessel, then
Neutralizer is added to neutralize, deionized water is added and is diluted to admittedly containing 33%-35%.
In some embodiments, base epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol S
At least one of type epoxy resin, novolac epoxy.
In some embodiments, chain extender is at least one of bisphenol-A and its derivative.
In some embodiments, organic solvent is toluene class and ketones solvent.
In some embodiments, the amine compounds containing active hydrogen are unitary secondary amine.In some embodiments, containing active
The amine compounds of hydrogen are ketimide, hydramine, alkylamine.
In some embodiments, neutralizer is organic acid or at least one of inorganic acid and its derivative.
Beneficial effect:
1, the graphene oxide after p-phenylenediamine is modified can be preferably dispersed in electrophoresis groove liquid, and compatibility is more preferable；
2, by the modified electrophoretic coating of modified graphene oxide, the anti-corrosive properties of coating are significantly improved.
Specific embodiment
The present invention is described in more detail below by embodiment.
Case study on implementation 1:
Step 1: the preparation of modified graphene oxide dispersion liquid
Preparation method: taking graphene oxide powder, and deionized water is then added, and ultrasonic disperse is sufficiently stirred 1 hour, system
Obtain the dispersion liquid of graphene oxide.Then graphene oxide dispersion is heated to 85 DEG C, slowly instills p-phenylenediamine, slowly stirs
It mixes, until powder all dissolves, then keeps the temperature 3 hours, deep purple solution is made.Then it is filtered, then uses deionization again
Water and dehydrated alcohol wash repeatedly, obtain modified graphene oxide aqueous dispersion, solid part 15%；
Specific additional amount is shown in Table 1:
| Component | Dosage (g) |
| Graphene oxide powder | 1 |
| Deionized water | 1250 |
| P-phenylenediamine | 5 |
| Total amount | 1256 |
Table 1: the dosage of modified graphene oxide dispersion liquid raw material
Step 2: the preparation of matrix resin:
In the reaction flask equipped with thermometer, blender and reflux condensing tube, 201 asphalt mixtures modified by epoxy resin of formula ratio are sequentially added
Rouge, bisphenol-A and first part's methyl iso-butyl ketone (MIBK).After charging, starts and stir and protected after reaction system is warming up to 120 DEG C
Temperature is risen to 150 DEG C after triphenylphosphine is added by temperature, and the reaction was continued at this temperature 1h, when reaction system epoxide equivalent reaches
When to theoretical value (EEW=1140.5), start to cool down；When system temperature is down to 100 DEG C or less, by N- methylethanolamine and ketone
Imines, second part methyl iso-butyl ketone (MIBK) are added in reaction system, are warming up to 120 DEG C again, the reaction was continued at this temperature
2h；Reaction system is cooled to 70 DEG C after reaction, obtains the matrix resin that final solid content is 85.0%.
Specific additional amount is shown in Table 2:
| Component | Dosage (g) |
| 201 epoxy resin (EEW=185) | 1480 |
| Bisphenol-A | 684 |
| Triphenylphosphine | 3 |
| Methyl iso-butyl ketone (MIBK) | 114 |
| N- methylethanolamine | 86 |
| Ketimide * | 174 |
| Methyl iso-butyl ketone (MIBK) | 390 |
| Total amount | 2931 |
* it is reacted and is prepared according to molar ratio 1:2 by diethylenetriamine and methyl iso-butyl ketone (MIBK), the solid content of final product are as follows:
73%
Table 2: the dosage of matrix resin raw material
Step 3: the preparation of curing agent:
4, the 4`- diphenyl methane of formula ratio is added in the reaction flask equipped with thermometer, blender and reflux condensing tube
Diisocyanate and dibutyl tin dilaurate, stirring starts that ethylene glycol monobutyl ether is added dropwise after being warming up to 60 DEG C, during dropwise addition
Cooled down with water-bath and control temperature no more than 65 DEG C, continues to react 2h at 80 DEG C after being added dropwise, it is anti-with standard di-n-butylamine
Titration analyzes remaining isocyanate group content in reaction system and it is different that methyl is added when remaining isocyanate group content is less than 0.2%
Butyl ketone is diluted, and obtains the totally-enclosed isocyanate crosslinking that final solid content is 80%.
Specific additional amount is shown in Table 3:
Table 3: the dosage of curing agent raw material
Step 4: the preparation of main body lotion:
What in the reaction flask equipped with blender prepared by the matrix resin of the second step preparation of addition formula ratio, third portion consolidates
Agent, ethylene glycol monobutyl ether start and stir and be uniformly mixed reaction system, and acetic acid, which is then added, and neutralize makes resin ion
Change, be eventually adding deionized water, emulsifying the organic solvent being evaporated under reduced pressure in removing lotion after 30min to get solid content is 35%
Main body lotion.
Specific additional amount is shown in Table 4:
| Component | Dosage (g) |
| The matrix resin of second step preparation | 500 |
| The curing agent of third step preparation | 200 |
| Ethylene glycol monobutyl ether | 8 |
| Acetic acid | 20 |
| Deionized water | 1001 |
| Total amount | 1729 |
Table 4: the dosage of main body emulsion materials
Step 5: the preparation of modified electrophoretic coating:
Electrophoretic coating is made according to following table cooperation, is subsequently placed in electrophoresis tank and cures 24 hours.Tank liquor temperature is in 32 DEG C of items
Under part, control voltage 200V, electrophoresis 30 seconds.Then it is baked 20 minutes at 200 DEG C, obtains the preferable paint film of paint film appearance.
Specific additional amount is shown in Table 5:
| Component | Dosage (g) |
| The main body lotion of 4th step preparation | 300 |
| The modified graphene oxide dispersion liquid of first step preparation | 6.6 |
| Black wash | 50 |
| Deionized water | 550 |
| Total amount | 906.6 |
Table 5: the dosage of modified electrophoretic coating raw material
Performance test:
Modified electrophoretic coating and the phosphatization plate after the coating electrophoresis of modified graphene oxide dispersion liquid is not added under the conditions of NSS
Salt fog performance is tested, relevant parameter is shown in Table 6.
| The modification electrophoretic coating of embodiment 1 | Modified graphene oxide dispersion liquid is not added | |
| Film thickness (μm) | 25 | 25 |
| Appearance | It is flat and smooth | It is flat and smooth |
| Neutral salt spray | >=1500 hours | >=1000 hours |
Table 6: experimental data
The antiseptic property of the modification electrophoretic coating of the embodiment of the present invention is compared with the antiseptic property of not modified electrophoretic coating
It is greatly enhanced.
The above statement is only preferred embodiment of the invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these also should be regarded as the protection model of invention
Within enclosing.
Claims (9)
1. a kind of preparation method of modified graphene oxide dispersion liquid, which comprises the following steps:
Then the deionized water of 1250 mass fractions is added in α 1, the graphene oxide powder for taking 1-5 mass fraction, stir 1h,
The dispersion liquid of graphene oxide is made；
α 2, the graphene oxide dispersion is heated to 80-90 DEG C, slowly instills the p-phenylenediamine of 5-8 mass fraction, slowly
Then stirring keeps the temperature 2-3h until powder all dissolves, deep purple solution is made；
α 3, the solution of the darkviolet is filtered, is then washed, is modified repeatedly with deionized water and dehydrated alcohol again
Graphene oxide aqueous dispersion.
2. a kind of modified electrophoretic coating, which is characterized in that the modified oxidized stone obtained including preparation method described in claim 1
Black alkene dispersion liquid and main body lotion.
3. a kind of modified electrophoretic coating according to claim 2, which is characterized in that the preparation method packet of the main body lotion
Include following steps:
β 1, small molecule base epoxy resin, chain extender, triphenylphosphine, organic solvent are added in the reaction vessel, in 120-160
Chain extending reaction is carried out between DEG C, obtains the macromolecular epoxy resin that epoxide equivalent is 1000-3000；
β 2, epoxide equivalent be 1000-3000 macromolecular epoxy resin in, be stirred continuously down and be warming up to 90-95 DEG C, addition contains
The amine compounds of active hydrogen are warming up to 115-125 DEG C, then keep the temperature 3 hours, obtain the main body asphalt mixtures modified by epoxy resin of amine modification after chain extension
Rouge；
Main body epoxy resin, the Blocked Isocyanate Curing Agents that amine is modified after addition chain extension in β 3, reaction vessel, are then added
Neutralizer neutralizes, and deionized water is added and is diluted to admittedly containing 33%-35%.
4. a kind of modified electrophoretic coating according to claim 3, which is characterized in that the base epoxy resin is bisphenol-A
At least one of type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, novolac epoxy.
5. a kind of modified electrophoretic coating according to claim 3, which is characterized in that the chain extender is bisphenol-A and its spreads out
At least one of biology.
6. a kind of modified electrophoretic coating according to claim 3, which is characterized in that the organic solvent is toluene class and ketone
Class solvent.
7. a kind of modified electrophoretic coating according to claim 3, which is characterized in that the amine compounds containing active hydrogen are
Unitary secondary amine.
8. a kind of modified electrophoretic coating according to claim 7, which is characterized in that the amine compounds containing active hydrogen are
At least one of ketimide, hydramine, alkylamine.
9. a kind of modified electrophoretic coating according to claim 3, which is characterized in that the neutralizer is organic acid or inorganic
At least one of acid and its derivative.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498411A (en) * | 2019-08-02 | 2019-11-26 | 贵州晟扬管道科技有限公司 | A kind of modified graphene oxide and processing technology |
| CN110760237A (en) * | 2019-10-16 | 2020-02-07 | 广州特种承压设备检测研究院 | Graphene conductive anticorrosive paint for subway stray current and preparation method thereof |
| CN111777919A (en) * | 2020-06-24 | 2020-10-16 | 东北大学 | Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry |
| CN111978818A (en) * | 2020-08-17 | 2020-11-24 | 上海金力泰化工股份有限公司 | Graphene oxide modified cathode electrophoresis primer and coating method thereof |
| CN112724792A (en) * | 2021-01-27 | 2021-04-30 | 南京锆时新材料科技有限公司 | Vehicle epoxy primer with excellent corrosion resistance and preparation method thereof |
| CN113583542A (en) * | 2021-08-25 | 2021-11-02 | 雅迪科技集团有限公司 | Corrosion-resistant graphene electrophoretic paint and preparation method thereof |
| CN113667378A (en) * | 2021-08-25 | 2021-11-19 | 雅迪科技集团有限公司 | Graphene electrophoretic paint and preparation method thereof |
| CN113755076A (en) * | 2021-09-30 | 2021-12-07 | 南通大学 | Preparation method of aromatic diamine modified graphene oxide epoxy resin coating |
| CN114456646A (en) * | 2022-03-01 | 2022-05-10 | 浩力森化学科技（江苏）有限公司 | Corrosion-resistant high-impact-resistance electrophoretic coating and preparation method thereof |
| CN114806348A (en) * | 2022-05-25 | 2022-07-29 | 江门市水电有限公司 | Coating composition and preparation method and application thereof |
| CN115340781A (en) * | 2022-09-05 | 2022-11-15 | 天津中航百慕新材料技术有限公司 | Graphene-basalt composition, coating and preparation method of coating |
| CN115724425A (en) * | 2022-09-30 | 2023-03-03 | 浙江铭孚金属涂装科技有限公司 | Preparation and use methods of functionalized graphene for modified cathode electrophoretic coating |
| CN116082917A (en) * | 2022-12-28 | 2023-05-09 | 湖州市吴兴区核源金属新材研究院 | Modified epoxy cathode electrophoretic paint and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110498411A (en) * | 2019-08-02 | 2019-11-26 | 贵州晟扬管道科技有限公司 | A kind of modified graphene oxide and processing technology |
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| CN110760237A (en) * | 2019-10-16 | 2020-02-07 | 广州特种承压设备检测研究院 | Graphene conductive anticorrosive paint for subway stray current and preparation method thereof |
| CN111777919A (en) * | 2020-06-24 | 2020-10-16 | 东北大学 | Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry |
| CN111978818A (en) * | 2020-08-17 | 2020-11-24 | 上海金力泰化工股份有限公司 | Graphene oxide modified cathode electrophoresis primer and coating method thereof |
| CN112724792A (en) * | 2021-01-27 | 2021-04-30 | 南京锆时新材料科技有限公司 | Vehicle epoxy primer with excellent corrosion resistance and preparation method thereof |
| CN113667378A (en) * | 2021-08-25 | 2021-11-19 | 雅迪科技集团有限公司 | Graphene electrophoretic paint and preparation method thereof |
| CN113583542A (en) * | 2021-08-25 | 2021-11-02 | 雅迪科技集团有限公司 | Corrosion-resistant graphene electrophoretic paint and preparation method thereof |
| CN113755076A (en) * | 2021-09-30 | 2021-12-07 | 南通大学 | Preparation method of aromatic diamine modified graphene oxide epoxy resin coating |
| CN114456646A (en) * | 2022-03-01 | 2022-05-10 | 浩力森化学科技（江苏）有限公司 | Corrosion-resistant high-impact-resistance electrophoretic coating and preparation method thereof |
| CN114456646B (en) * | 2022-03-01 | 2022-11-22 | 浩力森化学科技（江苏）有限公司 | Corrosion-resistant high-impact-resistance electrophoretic coating and preparation method thereof |
| CN114806348A (en) * | 2022-05-25 | 2022-07-29 | 江门市水电有限公司 | Coating composition and preparation method and application thereof |
| CN115340781A (en) * | 2022-09-05 | 2022-11-15 | 天津中航百慕新材料技术有限公司 | Graphene-basalt composition, coating and preparation method of coating |
| CN115724425A (en) * | 2022-09-30 | 2023-03-03 | 浙江铭孚金属涂装科技有限公司 | Preparation and use methods of functionalized graphene for modified cathode electrophoretic coating |
| CN116082917A (en) * | 2022-12-28 | 2023-05-09 | 湖州市吴兴区核源金属新材研究院 | Modified epoxy cathode electrophoretic paint and preparation method thereof |
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