CN110698887A - CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder - Google Patents

CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder Download PDF

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Publication number
CN110698887A
CN110698887A CN201911108487.4A CN201911108487A CN110698887A CN 110698887 A CN110698887 A CN 110698887A CN 201911108487 A CN201911108487 A CN 201911108487A CN 110698887 A CN110698887 A CN 110698887A
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China
Prior art keywords
graphite
ceo
drying
solution
composite powder
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Pending
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CN201911108487.4A
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Chinese (zh)
Inventor
王春雨
冯康
钟博
姜大海
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WEIHAI YUNSHAN TECHNOLOGY Co Ltd
Harbin Institute of Technology Weihai
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WEIHAI YUNSHAN TECHNOLOGY Co Ltd
Harbin Institute of Technology Weihai
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Publication of CN110698887A publication Critical patent/CN110698887A/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
    • 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
    • C09C3/06—Treatment with inorganic 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
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn
    • 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
    • C09D5/24—Electrically-conducting paints

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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)
  • Carbon And Carbon Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention relates to a surface modification process of nano-graphite, in particular to a method for attaching small and dispersedly distributed CeO on the surface of a graphite nano-sheet2Particle process, dispersed CeO for zinc-rich anticorrosive paint2The preparation method of the/graphite nano-sheet composite powder takes cerium nitrate as a cerium source, and CeO which is dispersed and distributed is loaded on the surface of the graphite nano-sheet by a hydrothermal method2Compared with the prior art, the method has simple technology and no equipment requirement, and the CeO on the graphite nanosheets2Uniform distribution, increased specific surface area of graphite nanosheet, and CeO2The modified composite powder can be used for anticorrosive material, photodegradation,Catalysis, battery electrodes, and the like.

Description

CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder
Technical Field
The invention relates to a surface modification process of a graphite material, in particular to a method for adhering and dispersing CeO on the surface of a graphite nanosheet2Particles to obtain a zinc-rich anticorrosive coating additive2A preparation method of graphite nano-sheet composite powder.
Background
The anticorrosive material has an important position in the scientific research field, and the research and development of the metal anticorrosive theory have a very important role in national economic development. At present, most of the mainly used anticorrosive materials are oily anticorrosive coatings, and the defects of heavy pollution, heavy weight and non-corrosion resistance exist. With the discovery of graphene, the excellent performance of carbon materials becomes an ideal anticorrosive material in the future, and research on the aspect has become a hot point of research.
One of the common methods for preparing the anticorrosive material from graphene is to uniformly mix graphene and slurry and coat the mixture on a metal substrate to prepare an anticorrosive coating. For example, Chinese patent with publication number 108864837A provides a double-bond modified graphene/polyvinylidene chloride heavy-duty anticorrosive paint and a preparation method thereof; chinese patent publication No. 108841211A provides an inorganic zinc-rich coating of modified graphene and a preparation method thereof. However, most of the used graphene is graphene oxide prepared by a Hummer method, and most of the graphene oxide prepared by the method has the defects of poor conductivity, low reduction degree and unsuitability for industrial production. The graphene prepared by a physical method can improve the defects to a certain extent, but the dispersibility of the material is reduced, and the corrosion resistance is poor. This conflict greatly limits the application of graphene anticorrosive materials.
Disclosure of Invention
Aiming at the problems of easy agglomeration and low corrosion resistance of graphene in the prior art, the invention provides CeO for a zinc-rich anticorrosive coating, which is simple and convenient to prepare, has low equipment requirement, enhances the dispersibility of graphene and improves the anticorrosive effect of the anticorrosive coating by adhering cerium oxide particles dispersed and distributed on the surface of a graphite nanosheet2A preparation method of graphite nano-sheet composite powder.
The invention is achieved by the following measures:
dispersion distribution CeO for zinc-rich anticorrosive paint2The preparation method of the graphite nanosheet composite powder is characterized by comprising the following steps:
the method comprises the following steps: dissolving cerium nitrate in an aqueous solution containing anhydrous sodium acetate until the solution is completely transparent; adding graphite nano-sheets into the solution;
step two: carrying out ultrasonic treatment until the graphite nanosheets are uniformly dispersed;
step three: putting the solution into a hydrothermal kettle, preserving the heat for 4 hours at the temperature of between 150 and 190 ℃, filtering, washing and drying to obtain CeO2Modified graphite nano-sheets.
The invention also comprises the step of pretreating the graphite nano-sheet, wherein the pretreatment is to put the graphite nano-sheet into concentrated sulfuric acid, concentrated nitric acid or other strong oxidizing acid for soaking and stirring.
The water washing process of the invention is to continue adding water after the suction filtration and then carrying out the suction filtration, repeatedly carrying out the water filtration for 3 to 5 times, or washing by using alcohol.
The drying is carried out by placing in room temperature air for natural drying, placing in an air furnace for slow heating for drying, or placing in a vacuum drying oven for drying or freeze drying, wherein the temperature is controlled below 100 ℃, and the time is based on complete drying of the powder.
Dispersed CeO obtained by the invention2The particles are attached to the surface of the graphite nanosheet and are distributed in a checkerboard manner. Compared with the prior art, the method has simple technology, no special equipment requirement and dispersed CeO on the nanosheets2The graphite nano-sheet has uniform adhesion, increases the specific surface area of the graphite nano-sheet, and can be used in various fields such as anticorrosive materials, photodegradation, battery electrodes and the like.
Description of the drawings:
FIG. 1 shows CeO dispersed in the present invention2An electron microscope image of the graphite nanosheet composite powder.
The specific implementation mode is as follows:
the invention is further illustrated by the following specific examples:
the invention provides a graphite nano-sheet surface adhered and dispersed CeO2Dissolving cerium nitrate in an aqueous solution containing anhydrous sodium acetate until the solution is completely transparent, adding graphite nanosheets into the solution, and carrying out ultrasonic treatment until the graphite nanosheets are uniformly dispersed; putting the solution into a hydrothermal tank, preserving the heat for 4 hours at the temperature of between 150 and 190 ℃, filtering, washing and drying to obtain CeO2The modified graphite nanosheet can be pretreated, for example, the graphite nanosheet is soaked in concentrated sulfuric acid, concentrated nitric acid or other strong oxidizing acid and stirred for a period of time; the water washing process is to continue adding a certain amount of water after the suction filtration and then carrying out the suction filtration, repeatedly carrying out the suction filtration for 3 to 5 times, and also using alcohol for washing; the drying process is to place the powder in room temperature air for natural drying or place the powder in an air furnace for slow heating drying or place the powder in a vacuum drying oven for drying or freeze drying, wherein the temperature is controlled below 100 ℃, and the time is based on complete drying of the powder.
Example 1:
dispersed granular CeO for anticorrosive paint2The preparation method of the modified graphite nanosheet composite powder comprises the following steps: adding 10ml of 0.6mol/L anhydrous sodium acetate solution and 0.15g of cerium nitrate into 80ml of water, stirring until the solution is completely transparent, adding 0.05g of graphite nanosheet, stirring for 10 minutes, putting the solution into an ultrasonic pool, carrying out ultrasonic treatment for 30 minutes, heating the solution in a hydrothermal reaction kettle to 190 ℃, keeping the temperature for 4 hours, carrying out pumping, water washing, and drying in a 65 ℃ drying box for 12 hours to obtain dispersed granular CeO2And graphite nano sheet composite material powder. The paint has good anticorrosion effect when being used in zinc-rich anticorrosive paint primer.
Example 2:
dispersed granular CeO for anticorrosive paint2Graphite nano sheet compositeThe preparation method of the composite powder comprises the following steps:
firstly, soaking graphite nano-sheets in strong oxidizing acid such as concentrated sulfuric acid or concentrated nitric acid for 4 hours, carrying out suction filtration, washing and drying treatment, then adding 10ml of 0.6mol/L anhydrous sodium acetate solution and 0.15g of cerium nitrate into 80ml of water, stirring until the solution is completely transparent, then adding 0.05g of graphite nano-sheets, stirring for 10 minutes, putting the graphite nano-sheets into an ultrasonic tank, carrying out ultrasonic treatment for 30 minutes, heating the graphite nano-sheets in a hydrothermal reaction kettle to 190 ℃, preserving heat for 4 hours, carrying out suction filtration washing, and drying in a 65 ℃ drying box for 12 hours to obtain dispersed granular CeO2And graphite nano sheet composite material powder.
CeO obtained by the invention2CeO attached to surface of graphite nanosheet composite material and distributed in a checkerboard-type dispersion manner2. The modified graphite nanosheet can improve the conductivity and hydrophobicity of the coating and improve the corrosion resistance of the zinc-rich anti-corrosion primer. Compared with the prior art, the method has simple technology and no equipment requirement, and the dispersed granular CeO on the nanosheets2The nano-sheet has uniform adhesion, increases the specific surface area of the nano-sheet, and can be used in various fields such as anticorrosive materials, photodegradation, catalysis, battery electrodes and the like.

Claims (4)

1. Dispersion distribution CeO for zinc-rich anticorrosive paint2The preparation method of the graphite nanosheet composite powder is characterized by comprising the following steps:
the method comprises the following steps: dissolving cerium nitrate in an aqueous solution containing anhydrous sodium acetate until the solution is completely transparent; adding graphite nano-sheets into the solution;
step two: carrying out ultrasonic treatment until the graphite nanosheets are uniformly dispersed;
step three: putting the solution into a hydrothermal kettle, preserving the heat for 4 hours at the temperature of between 150 and 190 ℃, filtering, washing and drying to obtain CeO2Modified graphite nano-sheets.
2. Dispersed CeO for zinc-rich anticorrosive paint according to claim 12The preparation method of the graphite nano-sheet composite powder is characterized by also comprising the step of pretreating the graphite nano-sheetThe treatment is to put the graphite nano-sheet into concentrated sulfuric acid, concentrated nitric acid or other strong oxidizing acid to be soaked and stirred.
3. Dispersed CeO for zinc-rich anticorrosive paint according to claim 12The preparation method of the graphite nano sheet composite powder is characterized in that the drying is natural drying in room temperature air or slow heating drying in an air furnace or drying in a vacuum drying oven or freeze drying, the temperature is controlled below 100 ℃, and the time is based on complete drying of the powder.
4. Dispersed CeO for zinc-rich anticorrosive paint according to claim 12The preparation method of the graphite nanosheet composite powder is characterized by comprising the following steps of: adding 10ml of 0.6-2 mol/L anhydrous sodium acetate solution and 0.15-0.5 g of cerium nitrate into 80ml of water, stirring until the solution is completely transparent, adding 0.05-0.5 g of graphite nanosheet, stirring for 10 minutes, putting the solution into an ultrasonic pool, performing ultrasonic treatment for 30 minutes, heating the solution in a hydrothermal reaction kettle to 190 ℃, preserving heat for 4 hours, performing suction filtration washing, and drying in a 65 ℃ drying box for 12 hours to obtain CeO2Graphite nano sheet composite powder.
CN201911108487.4A 2019-08-14 2019-11-13 CeO for zinc-rich anticorrosive paint2Preparation method of graphite nanosheet composite powder Pending CN110698887A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111205693A (en) * 2020-02-20 2020-05-29 重庆市城投路桥管理有限公司 Anti-corrosion primer for bridge and preparation method thereof
CN111334251A (en) * 2020-04-09 2020-06-26 哈尔滨工业大学（威海） Preparation method and application of graphite nanosheet multiphase carbon compound

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CN103066292A (en) * 2013-01-30 2013-04-24 同济大学 Grapheme/rare earth oxide nanometer composite material and preparation method and application thereof
CN105255446A (en) * 2015-11-06 2016-01-20 安徽理工大学 Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof
CN105948032A (en) * 2016-07-04 2016-09-21 烟台市烯能新材料股份有限公司 Method for etching multilayer graphene
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CN106744921A (en) * 2016-12-29 2017-05-31 哈尔滨工业大学（威海） The TiO of electric heating film2The preparation method of/graphite nano plate composite granule

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CN103066292A (en) * 2013-01-30 2013-04-24 同济大学 Grapheme/rare earth oxide nanometer composite material and preparation method and application thereof
CN105255446A (en) * 2015-11-06 2016-01-20 安徽理工大学 Reduced graphene oxide and nano cerium oxide composite microwave absorbing material and preparation method thereof
CN105948032A (en) * 2016-07-04 2016-09-21 烟台市烯能新材料股份有限公司 Method for etching multilayer graphene
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CN106744921A (en) * 2016-12-29 2017-05-31 哈尔滨工业大学（威海） The TiO of electric heating film2The preparation method of/graphite nano plate composite granule

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111205693A (en) * 2020-02-20 2020-05-29 重庆市城投路桥管理有限公司 Anti-corrosion primer for bridge and preparation method thereof
CN111334251A (en) * 2020-04-09 2020-06-26 哈尔滨工业大学（威海） Preparation method and application of graphite nanosheet multiphase carbon compound

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Application publication date: 20200117