CN111777919A - Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry - Google Patents

Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry Download PDF

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Publication number
CN111777919A
CN111777919A CN202010586190.5A CN202010586190A CN111777919A CN 111777919 A CN111777919 A CN 111777919A CN 202010586190 A CN202010586190 A CN 202010586190A CN 111777919 A CN111777919 A CN 111777919A
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graphene
temperature
mechanochemistry
anticorrosive paint
preparation
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孟凡帝
栾浩
刘莉
郑宏鹏
崔宇
王福会
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Northeastern University China
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Northeastern University China
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Priority to CN202410448233.1A priority patent/CN118185430A/en
Publication of CN111777919A publication Critical patent/CN111777919A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation method of a resinified graphene anticorrosive paint based on high-temperature mechanochemistry, which comprises the following steps: taking graphene or graphene oxide, and adding phenylenediamine into the graphene or graphene oxide aqueous solution for modification pretreatment; adding organic resin and a solvent, treating by adopting a high-temperature mechanochemical method, centrifuging, filtering, and drying the obtained solution to obtain resinified graphene; mixing the resinated graphene with organic resin, diluent and additive, and mechanically stirring to obtain a component A; and uniformly mixing the component A and the component B to obtain the resinated graphene anticorrosive paint. The chemical reaction of graphene and organic resin can be realized by a high-temperature mechanochemical technology; the resinated graphene can be uniformly dispersed in organic resin, has high bonding strength with a film forming substance, reduces the hole defects in the coating, and improves the barrier property and the mechanical property of the coating, thereby obtaining better corrosion resistance.

Description

Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry
Technical Field
The invention relates to the field of organic anticorrosive coatings, in particular to a preparation method of a resinated graphene anticorrosive coating based on high-temperature mechanochemistry.
Background
Graphene is a new choice for shielding fillers in anticorrosive coatings due to its high specific surface area, excellent permeation resistance, good thermal stability and other properties, and has attracted extensive attention of researchers in the anticorrosive field. However, the graphene filler is extremely easy to agglomerate due to the high surface energy and has poor compatibility with the oily organic coating, and the expected use effect and protective capability of the graphene anticorrosive coating cannot be achieved.
At present, chemical grafting methods are mostly adopted for modification researches of graphene and graphene oxide, and graphene and organic substances are connected in a covalent bond or non-covalent bond mode through a certain bridging agent so as to solve the problems of dispersion of graphene and compatibility of graphene and organic coatings, and the operation is complex and is often difficult to be used in practical production. Therefore, the development of the modified graphene anticorrosive paint which is simple to synthesize, can obtain good dispersity and compatibility and is expected to be produced in large quantities has very strong practical significance.
Disclosure of Invention
The invention aims to provide a method for preparing an anticorrosive coating by chemically resinating graphene oxide by using high-temperature mechanochemistry, which not only realizes good dispersity of graphene, but also has excellent compatibility and bonding strength with resin in an organic coating by using the high-temperature mechanochemistry technology, thereby obtaining the anticorrosive coating with good barrier property and mechanical property.
The technical scheme of the invention is as follows:
a preparation method of a resinified graphene anticorrosive paint based on high-temperature mechanochemistry is characterized by comprising the following specific steps:
(1) taking graphene or graphene oxide, and adding phenylenediamine into the graphene or graphene oxide aqueous solution for modification pretreatment;
(2) taking the pretreated graphene or graphene oxide in the step (1), adding organic resin and a solvent, treating by adopting a high-temperature mechanochemical method, and centrifuging, filtering and drying the obtained solution to obtain resinified graphene;
(3) mixing the resinated graphene in the step (2) with organic resin, diluent and additive, and mechanically stirring to obtain a component A;
(4) and uniformly mixing the component A and the component B to obtain the resinated graphene anticorrosive paint.
In the step (1), the phenylenediamine can be one or more of three isomers of phenylenediamine, m-phenylenediamine and p-phenylenediamine.
The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry has the preferable scheme that in the step (1), the modification pretreatment is to mechanically stir a mixture at 80-95 ℃ for 3-7 hours, and then to obtain the pretreated graphene after taking out and carrying out centrifugation and suction filtration.
The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry has the preferable scheme that in the step (2), the organic resin is one of, but not limited to, epoxy resin, castor oil, acrylic resin or alkyd resin. The mass ratio of the organic resin to the graphene is 1-100: 1.
the preferable scheme of the preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry is that in the step (2), the high-temperature mechanochemistry is high-energy mechanical ball milling in which a mixture is reacted at the reaction temperature of 30-200 ℃, the reaction time is 1-10 hours, and the ball milling rotation speed is 200-800 rpm.
The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry has the preferable scheme that in the step (2), the solvent comprises but is not limited to one or more of xylene, n-butanol and toluene.
The preferable scheme of the preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry is that in the step (3), the mass ratio of the resinated graphene to the organic resin to the diluent is 0.001-0.05:1: 0.1-0.5.
The preferable scheme of the preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry is that in the step (4), the component B curing agent comprises amine, ether or anhydride curing agent, and the mass ratio of the component B to the organic resin in the component A is 0.1-1: 1.
The invention has the beneficial effects that: according to the preparation method of the resinated graphene anticorrosive paint based on high-temperature mechanochemistry, the chemical reaction of graphene and organic resin can be directly realized through a high-temperature mechanochemistry technology; the resinated graphene can be uniformly dispersed in organic resin, has high bonding strength with a film forming substance, reduces the hole defects in the coating, and improves the barrier property and the mechanical property of the coating, thereby obtaining better corrosion resistance. The graphene oxide in the coating product is small in addition amount, good coating anticorrosion effect and compactness can be obtained with low addition amount, and the coating product can be applied to oil pipelines, ships, ocean platforms and other equipment, and plays roles in anticorrosion, wear resistance and protection of base metal.
Drawings
FIG. 1 is an infrared spectrum of graphene and washed resinated graphene powder;
FIG. 2 shows the contact angle test results of graphene and washed resinated graphene;
FIG. 3 shows a water absorption test curve of a common graphene epoxy coating and a resinated graphene coating.
Detailed Description
The present invention is further described in the following examples, which are intended to be illustrative of the best mode of carrying out the invention and are not intended to limit the scope of the invention in any way.
Example 1
In this embodiment, the preparation method of the resinated graphene anticorrosive coating based on high-temperature mechanochemistry comprises the following specific steps:
(1) taking graphene or graphene oxide, and adding phenylenediamine into the graphene or graphene oxide aqueous solution for modification pretreatment;
(2) taking the pretreated graphene or graphene oxide in the step (1), adding organic resin and a solvent, treating by adopting a high-temperature mechanochemical method, and centrifuging, filtering and drying the obtained solution to obtain resinified graphene;
(3) mixing the resinated graphene in the step (2) with organic resin, diluent and additive, and mechanically stirring to obtain a component A;
(4) and uniformly mixing the component A and the component B to obtain the resinated graphene anticorrosive paint. In the step (1), the phenylenediamine can be one or more of three isomers of o-phenylenediamine, m-phenylenediamine and p-phenylenediamine, and preferably m-phenylenediamine is used as a reaction substance.
In the step (1), the modification pretreatment is to mechanically stir the mixture for 3-7 hours at 80-95 ℃, take out the mixture, and then perform centrifugation and suction filtration to obtain pretreated graphene, wherein the preferred range is 90-95 ℃ and the mechanical stirring is 6-7 hours.
In the step (2), the organic resin is but not limited to one of epoxy resin, castor oil, acrylic resin or alkyd resin, and the mass ratio of the organic resin to the graphene is 1-100: 1, in the embodiment, epoxy resin E-44 is selected, and the preferable mass ratio of the epoxy resin to the graphene is 10: 1.
in the step (2), the high-temperature mechanochemical method is high-energy mechanical ball milling in which the mixture reacts at the reaction temperature of 30-200 ℃, the reaction time of 1-10 hours and the ball milling rotation speed of 200-800 rpm. The preferable conditions are a reaction temperature of 150 ℃, a reaction time of 5 hours, and a ball milling rotation speed of 600 rpm.
In the step (2), the solvent includes but is not limited to one or more of xylene, n-butanol and toluene.
In the step (3), the mass ratio of the resinated graphene to the organic resin to the diluent is 0.001-0.05:1: 0.1-0.5. Preferably, the mass ratio of the resinated graphene to the organic resin to the diluent is 0.005:1: 0.3.
In the step (4), the curing agent of the component B comprises an amine, ether or anhydride curing agent, preferably, the component B is selected from a polyamide TY-650 curing agent, and the mass ratio of the component B to the organic resin in the component A is 0.8: 1.
The infrared spectrum test of the resinated graphene oxide powder of example 1 and the conventional graphene oxide was performed, and the results are shown in fig. 1. The result shows that the existence of the epoxy functional group after multiple times of washing proves that the graphene oxide and the epoxy resin realize chemical reaction and have good bonding strength and compatibility.
Fig. 2 is contact angle data of resinated graphene oxide and graphene oxide, and the result shows that lipophilicity of graphene is greatly enhanced after high-temperature mechanical chemical treatment.
Fig. 3 is a water absorption curve with 0.5 wt% of resinated graphene oxide coating added and graphene oxide epoxy coating soaked in 3.5 wt.% NaCl. The result shows that the water absorption capacity of the resinated graphene oxide coating is lower, and the coating has more excellent barrier property.

Claims (8)

1. A preparation method of a resinified graphene anticorrosive paint based on high-temperature mechanochemistry is characterized by comprising the following specific steps:
(1) taking graphene or graphene oxide, and adding phenylenediamine into the graphene or graphene oxide aqueous solution for modification pretreatment;
(2) taking the pretreated graphene or graphene oxide in the step (1), adding organic resin and a solvent, treating by adopting a high-temperature mechanochemical method, and centrifuging, filtering and drying the obtained solution to obtain resinified graphene;
(3) mixing the resinated graphene in the step (2) with organic resin, diluent and additive, and mechanically stirring to obtain a component A;
(4) and uniformly mixing the component A and the component B to obtain the resinated graphene anticorrosive paint.
2. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (1), the phenylenediamine can be one or more of three isomers of phenylenediamine, m-phenylenediamine and p-phenylenediamine.
3. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (1), the modification pretreatment is to mechanically stir the mixture for 3-7 hours at 80-95 ℃, take out, and then carry out centrifugation and suction filtration to obtain the pretreated graphene.
4. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (2), the organic resin is, but not limited to, one of epoxy resin, castor oil, acrylic resin or alkyd resin. The mass ratio of the organic resin to the graphene is 1-100: 1.
5. the preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (2), the high-temperature mechanochemical method is high-energy mechanical ball milling in which the mixture reacts at the reaction temperature of 30-200 ℃, the reaction time of 1-10 hours and the ball milling rotation speed of 200-800 rpm.
6. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (2), the solvent includes but is not limited to one or more of xylene, n-butanol and toluene.
7. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (3), the mass ratio of the resinated graphene to the organic resin to the diluent is 0.001-0.05:1: 0.1-0.5.
8. The preparation method of the modified graphene anticorrosive paint based on high-temperature mechanochemistry as claimed in claim 1, characterized in that: in the step (4), the curing agent of the component B comprises amine, ether or anhydride curing agent, and the mass ratio of the component B to the organic resin in the component A is 0.1-1: 1.
CN202010586190.5A 2020-06-24 2020-06-24 Preparation method of resinified graphene anticorrosive paint based on high-temperature mechanochemistry Pending CN111777919A (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN114806346A (en) * 2022-04-01 2022-07-29 哈尔滨工程大学 High-temperature mechanochemical modified titanium dioxide anticorrosive coating and preparation method thereof
CN116120764A (en) * 2023-02-20 2023-05-16 诺比侃人工智能科技(成都)股份有限公司 Amino modified graphene and preparation method and application thereof

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CN109111782A (en) * 2018-07-19 2019-01-01 浩力森化学科技（江苏）有限公司 The preparation method of modified graphene oxide dispersion liquid and modified electrophoretic coating
CN109423160A (en) * 2017-07-13 2019-03-05 山东欧铂新材料有限公司 It is a kind of to contain graphene/epoxy resin composite material resin anti-corrosive paint and preparation method thereof

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CN109423160A (en) * 2017-07-13 2019-03-05 山东欧铂新材料有限公司 It is a kind of to contain graphene/epoxy resin composite material resin anti-corrosive paint and preparation method thereof
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114806346A (en) * 2022-04-01 2022-07-29 哈尔滨工程大学 High-temperature mechanochemical modified titanium dioxide anticorrosive coating and preparation method thereof
CN116120764A (en) * 2023-02-20 2023-05-16 诺比侃人工智能科技(成都)股份有限公司 Amino modified graphene and preparation method and application thereof

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