CN107964097B - Preparation method and application of ternary nanocomposite of reduced graphene oxide, ferroferric oxide and polyaniline - Google Patents

Preparation method and application of ternary nanocomposite of reduced graphene oxide, ferroferric oxide and polyaniline Download PDF

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CN107964097B
CN107964097B CN201711440114.8A CN201711440114A CN107964097B CN 107964097 B CN107964097 B CN 107964097B CN 201711440114 A CN201711440114 A CN 201711440114A CN 107964097 B CN107964097 B CN 107964097B
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朱爱萍
史萍萍
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Yangzhou University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/02—Polyamines
    • C08G73/026—Wholly aromatic polyamines
    • C08G73/0266—Polyanilines or derivatives thereof
    • 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
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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    • 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
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2265—Oxides; Hydroxides of metals of iron
    • C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/011—Nanostructured additives

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Abstract

A preparation method and application of a ternary nano composite material of reduced graphene oxide, ferroferric oxide and polyaniline relate to the technical field of preparation of functional nano anti-corrosion composite materials for water-based anti-corrosion coating materials. Graphene oxide, ferroferric oxide and aniline are subjected to reduction reaction and oxidation polymerization reaction to form the nanocomposite material with electron transfer interaction among ternary interfaces, and the feeding mass ratio of the graphene oxide to the ferroferric oxide to the aniline is 3: 4-7: 6-24. The constructed ternary nano composite material is filled in water-based paint resin to prepare the water-based nano paint, and the water-based paint coating has more excellent corrosion resistance compared with a paint not filled with the nano composite material. The efficient barrier property of the ternary nano composite material and the passivation function of the metal surface are realized.

Description

Preparation method and application of ternary nanocomposite of reduced graphene oxide, ferroferric oxide and polyaniline
Technical Field
The invention relates to the technical field of preparation of functional nano anticorrosive composite materials for water-based anticorrosive coating materials.
Background
Corrosion of a metal refers to the chemical, electrochemical or physical interaction between the metal and the ambient medium in which it is located, causing deterioration and destruction of the metal. The corrosion of metal brings huge loss to the whole society, and how to reduce the corrosion of metal becomes a problem which is concerned by people. Statistically, the total amount of steel damaged by corrosion is more than 1/3 every year all over the world, and the total amount of metal corrosion products which cannot be recycled reaches 1/9, which causes huge waste of resources. On the other hand, the corrosion of metal equipment can bring great potential safety hazard to production and life, for example, chemical equipment is corroded to easily cause equipment perforation to cause chemical raw material leakage, thereby causing explosion and toxic substance diffusion, and causing great harm to production workers, surrounding residents and the environment. Therefore, researchers in various countries seek to slow down and prevent the occurrence of corrosion.
At present, the metal corrosion prevention method which is economical and applicable is to coat the metal surface with the corrosion prevention coating so as to prolong the service life of the metal. The traditional design principle of the anticorrosive paint mostly adopts zinc-rich primer, the design concentration of zinc powder of the zinc-rich primer is not lower than 70 percent (weight) of the anticorrosive paint, so that the sacrificial anode can protect a cathode (metal substrate), or toxic heavy metals such as chromium, nickel and the like are adopted to form a compact metal complex on the surface of the metal substrate, so that the anticorrosion is realized. The scheme not only causes excessive consumption of resources, but also brings toxic substances to the environment. To date, no ideal method for overcoming the problems exists, and therefore, the development of a green and efficient anticorrosive filling material to endow paint with ideal anticorrosive performance is always the research direction in the scientific and technical fields.
The conductive polymer such as polyaniline has reversible redox activity, can continuously passivate the metal surface, is considered as a green anticorrosive material, and has great application value in the anticorrosive field. However, polyaniline loses electrochemical activity when the pH is more than 5, and loses electrochemical corrosion protection effect in the application occasions of high pH environments (pH is more than or equal to 7) such as oceans, which limits the popularization and application of polyaniline in the field of corrosion protection to a great extent.
Due to the advantages of unique nanosheet morphology, large specific surface area, high-efficiency barrier and the like, graphene has attracted extensive research interest in the application of anticorrosive coatings in recent years. However, graphene is difficult to disperse in water-based paint resin, which limits the popularization and application of graphene anticorrosive paint.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a reduced graphene oxide, ferroferric oxide and polyaniline ternary nanocomposite material with efficient corrosion resistance.
The preparation method comprises the following steps: the nanometer composite material with the electron transfer interaction between three interfaces is formed by the reduction reaction and the oxidation polymerization reaction of graphene oxide, ferroferric oxide and aniline, and is characterized in that: the feeding mass ratio of the graphene oxide to the ferroferric oxide to the aniline is 3: 4-7: 6-24.
Within the range of the charge ratio, electron transfer interaction is formed between the composite material interfaces to strengthen the redox activity of the polyaniline, and the redox activity is still maintained particularly in neutral or alkaline environments. The water-based nano coating is prepared by filling the constructed ternary nano composite material into water-based coating resin, and the water-based coating has more excellent corrosion resistance compared with a coating not filled with the nano composite material. The efficient barrier property of the ternary nano composite material and the passivation function of the metal surface are realized.
The preparation method comprises the following steps: firstly, graphene oxide and ferroferric oxide are dispersed into water under the ultrasonic condition, aniline is added, and then the graphene oxide and the ferroferric oxide react at the temperature of 95 ℃ to obtain aniline-reduced graphene oxide (rGO) loaded Fe3O4A binary composite material; after the reaction is finished, adjusting the pH value of the reaction system to 1-2, and adding an initiator ammonium persulfate to carry out rGO (graphene oxide) Fe loading3O4Oxidative polymerization of surface aniline; after 24 hours of reaction, rGO/Fe is obtained3O4the/PANI ternary nano composite material is washed by ethanol and water for three times respectively, and then dried to obtain the powdery ternary nano composite material.
The invention also aims to provide the application of the ternary nanocomposite of graphene oxide, ferroferric oxide and polyaniline.
The ternary nano composite material is easily dispersed in a water-based paint resin matrix after sanding to prepare the waterborne nano paint.
The key technology and the beneficial effects of the invention are as follows:
(1) the ternary nano composite material strengthens the redox activity of polyaniline by forming electron transfer interaction between ternary interfaces, and still maintains the redox activity in neutral or even alkaline environment;
(2) compared to rGO and Fe3O4The ternary nano composite material is easily dispersed in water-based paint resin after sanding to prepare the water-based nano paint, and the prepared water-based nano coating not only has excellent mechanical property, but also has excellent chemical medium resistance and salt spray resistance;
(3) the ternary nano composite material can well play roles in high-efficiency barrier property and metal surface passivation.
The mass filling amount of the ternary nano composite material in the water-based nano coating is 1-3%. Under the condition of the proportion, the ternary nano composite material can be well dispersed in the water-based paint under the premise of ensuring the corrosion resistance, and can obtain excellent corrosion resistance.
Drawings
FIG. 1 is rGO/Fe prepared in comparative example3O4Transmission electron microscopy of the composite.
FIG. 2 shows rGO/Fe obtained in example 23O4Transmission electron micrograph of the/PANI composite material.
FIG. 3 is rGO/Fe3O4CV diagram of the/PANI ternary nanocomposite material in different pH mediums.
Detailed Description
Firstly, a preparation process:
example 1:
1. preparation of rGO/Fe3O4the/PANI ternary nano composite material comprises the following components:
weighing 0.279g of graphite oxide (rGO) and 0.372g of ferroferric oxide (Fe)3O4) Dispersed in 150ml of distilled water, transferred to a 250ml three-neck flask, and ultrasonically stirred for 30 min. Then adding 0.558g of aniline, and heating for 4 hours in a water bath kettle at the constant temperature of 95 ℃; and then cooling the water bath to 0-5 ℃, adding acetic acid, and adjusting the pH value of the mixed system to 1.
1.824g of initiator Ammonium Persulfate (APS) was weighed out and dissolved in 50ml of an aqueous solution, and transferred to a constant pressure dropping funnel, and slowly dropped into the system for 60 min. The reaction was carried out for 24h under ice-bath conditions.
After the reaction is finished, washing the product with ethanol and water, and finally carrying out vacuum drying and grinding at 80 ℃ to prepare rGO/Fe3O4the/PANI (3: 4: 6) ternary nano composite material is characterized in that the feeding mass ratio of the graphene oxide, the ferroferric oxide and the aniline is 3:4: 6.
2. Preparing a water-based anticorrosive paint:
15g of water-based acrylic resin and 1g of amino resin curing agent are weighed and added into a 100ml beaker, and the mixture is fully and uniformly stirred to obtain the water-based acrylic varnish.
Weighing 3.45g of the sanded ternary nanocomposite, wherein the solid content of the ternary nanocomposite is 13%, adding the ternary nanocomposite into water-based paint resin, stirring uniformly, and adding an amino resin curing agent to obtain the water-based nano paint, wherein the content of the nanocomposite in the coating is 3 wt%.
Example 2:
1. preparation of rGO/Fe3O4the/PANI ternary nano composite material comprises the following components:
0.279g of graphite oxide and 0.651g of ferroferric oxide are weighed and dispersed in 150ml of distilled water, transferred into a 250ml three-neck flask, and ultrasonically stirred for 30 min. Then adding 0.558g of aniline, and heating for 4 hours in a water bath kettle at the constant temperature of 95 ℃; and then cooling the water bath to 0-5 ℃, adding acetic acid, and adjusting the pH value of the mixed system to 1.
1.824g of initiator APS was weighed out and dissolved in 50ml of aqueous solution, transferred to a constant pressure dropping funnel and slowly added dropwise to the system over a period of 60 min. The reaction was carried out for 24h under ice-bath conditions.
After the reaction is finished, washing the product with ethanol and water, and finally carrying out vacuum drying and grinding at 80 ℃ to obtain rGO/Fe3O4the/PANI ternary nano composite material is characterized in that the feeding mass ratio of the graphene oxide, the ferroferric oxide and the aniline is 3:7: 6.
2. Preparing a water-based anticorrosive paint:
using rGO/Fe3O4The other procedure is the same as that of step 2 in example 1 to obtain the water-based nano anticorrosive paint.
Example 3:
1. preparation of rGO/Fe3O4the/PANI ternary nano composite material comprises the following components:
0.279g of graphite oxide and 0.651g of ferroferric oxide are weighed and dispersed in 150ml of distilled water, transferred into a 250ml three-neck flask, and ultrasonically stirred for 30 min. Then adding 3.348g of aniline, and heating for 4 hours in a water bath kettle at the constant temperature of 95 ℃; and then cooling the water bath to 0-5 ℃, adding acetic acid, and adjusting the pH value of the mixed system to 1.
4.5g of initiator APS is weighed out and dissolved in 50ml of aqueous solution, and transferred to a constant pressure dropping funnel, and slowly dropped into the system, wherein the dropping time is 60 min. The reaction was carried out for 24h under ice-bath conditions.
After the reaction is finished, washing the product with ethanol and water, and finally carrying out vacuum drying and grinding at 80 ℃ to obtain rGO/Fe3O4the/PANI ternary nano composite material is characterized in that the feeding mass ratio of the graphene oxide, the ferroferric oxide and the aniline is 3:7: 12.
2. Preparing a water-based anticorrosive paint:
using rGO/Fe3O4The other procedure is the same as that of step 2 in example 1 to obtain the water-based nano anticorrosive paint.
Example 4:
1. preparation of rGO/Fe3O4the/PANI ternary nano composite material comprises the following components:
0.279g of graphite oxide and 0.651g of ferroferric oxide are weighed and dispersed in 150ml of distilled water, transferred into a 250ml three-neck flask, and ultrasonically stirred for 30 min. Adding 6.696g aniline, and heating in a water bath kettle at 95 deg.C for 4 h; and then cooling the water bath to 0-5 ℃, adding acetic acid, and adjusting the pH value of the mixed system to 1.
9.0g of initiator APS is weighed out and dissolved in 50ml of aqueous solution, and transferred to a constant pressure dropping funnel, and slowly dropped into the system, wherein the dropping time is 60 min. The reaction was carried out for 24h under ice-bath conditions.
After the reaction is finished, washing the product with ethanol and water, and finally carrying out vacuum drying and grinding at 80 ℃ to obtain rGO/Fe3O4the/PANI (3: 7: 24) ternary nanocomposite.
Step 2, preparing the water-based anticorrosive paint
Filled rGO/Fe3O4The other procedure is the same as that of step 2 in example 1 to obtain the water-based nano anticorrosive paint.
Comparative example:
step 1, preparing rGO/Fe3O4Binary nanocomposite
0.279g of graphite oxide and 0.651g of ferroferric oxide are weighed and dispersed in 150ml of distilled water, and transferred toIn a 250ml three-neck flask, stir by ultrasound for 30 min. 0.279g of aniline was then added and the mixture was heated in a water bath at 95 ℃ for 4 hours. After the reaction is finished, washing the product with ethanol and water, and finally carrying out vacuum drying and grinding at 80 ℃ to obtain rGO/Fe3O4(3: 7) the binary nano composite material, wherein the feeding mass ratio of the graphene oxide to the ferroferric oxide is 3: 7.
2. Preparing a water-based anticorrosive paint:
using rGO/Fe3O4(3: 7) preparing the water-based nano anticorrosive paint by the same steps as the step 2 of the example 1.
Secondly, application:
four groups of treated, clean surfaced tinplate or iron bar samples were prepared for parallel testing.
The aqueous anticorrosive coatings prepared in the above examples 2 and 1 comparative examples are respectively and uniformly coated on the treated galvanized iron sheet or iron bar with clean surface, and cured at 175 ℃ for 25-30 min to form aqueous nano coatings.
And thirdly, analyzing and comparing the test groups.
FIG. 1 is rGO/Fe prepared in comparative example3O4Transmission electron microscopy of the composite.
As can be seen from FIG. 1, Fe3O4The nanoparticles are supported on reduced graphene oxide sheets.
FIG. 2 shows rGO/Fe obtained in example 23O4Transmission electron micrograph of the/PANI composite material.
As can be seen from FIG. 2, Fe3O4A polyaniline shell layer is coated around the nano particles, and a layer of polyaniline grows on the surface of the reduced graphene oxide to form rGO/Fe3O4the/PANI ternary nano composite material can form electron transfer mutual lease between interfaces.
FIG. 3 is rGO/Fe3O4CV diagram of the/PANI ternary nanocomposite material in different pH mediums. As can be seen in the figure, rGO/Fe3O4the/PANI composite material not only has stronger oxidation-reduction activity in an acid environment, but also has oxygen under neutral and alkaline conditionsThe redox activity is that the electrochemical activity of the polyaniline is effectively enhanced and expanded to be neutral or even alkaline due to the electron transfer interaction formed between the interfaces of the ternary nano composite material.
The products with nanocoating obtained in the comparative example and those with nanocoating obtained in example 2 were immersed in solutions with different pH (1, 7 and 9 respectively) for 21 days for electrochemical ac impedance tests, wherein the results of corrosion potential and corrosion current are given in the following table:
Figure DEST_PATH_IMAGE001
from the above table, it can be seen that, compared with the aqueous coating filled with the ternary nanoparticles, the aqueous coating filled with the binary nanoparticles has lower corrosion potential, higher corrosion current and poorer corrosion resistance in each medium.
The electrochemical ac impedance test was performed by soaking the product with the aqueous nanocoating obtained in the comparative example and the product with the aqueous nanocoating obtained in example 2 in solutions with different pH (1, 7, 9), respectively, and the results are shown in the following table:
Figure DEST_PATH_IMAGE002
*|Z|0.1Hzthe unit is omega cm2
As can be seen from the above table, compared to rGO/Fe3O4，rGO/Fe3O4the/PANI filled water-based nano coating has more excellent corrosion resistance in acid, neutral and alkaline environments.
The value (| Z |) at low frequency (0.1Hz) can well characterize the corrosion protection properties of the coating. L Z | L0.1HzThe larger the coating, the better the corrosion resistance of the coating. When/| Z |0.1HzBelow 1.0E6 means loss of corrosion protection properties.
The product with the water-based nano coating obtained in the comparative example and the product with the water-based nano coating obtained in the implementation 2 are respectively subjected to various mechanical property index tests, and the results are shown in the following table:
Figure DEST_PATH_IMAGE003
note: the adhesive force grades are from strong to weak: level 0; grade 1; 2, level; 3, grade; and 4, level.
The product with the water-based nano coating obtained in the comparative example and the product with the water-based nano coating obtained in the implementation 2 are respectively subjected to medium resistance and salt spray resistance performance index tests, and the results are shown in the following table:
Figure DEST_PATH_IMAGE004
as can be seen from the above table, the aqueous nano-coating formed by the ternary nanocomposite has excellent mechanical properties, medium resistance and salt spray resistance.
In addition, tests have shown that the samples obtained in examples 1, 3, 4 and 2 have comparable properties.

Claims (1)

1. The application of the ternary nanocomposite of reduced graphene oxide, ferroferric oxide and polyaniline is characterized in that: dispersing the ternary nano composite material into a water-based paint resin matrix after sanding to prepare a water-based nano paint;
the preparation process comprises the following steps:
1) preparation of rGO/Fe3O4the/PANI ternary nano composite material comprises the following components:
weighing 0.279g of graphite oxide and 0.651g of ferroferric oxide, dispersing in 150ml of distilled water, transferring to a 250ml three-neck flask, ultrasonically stirring for 30min, then adding 0.558g of aniline, and heating in a water bath kettle at the temperature of 95 ℃ for 4h at constant temperature; then cooling the water bath to 0-5 ℃, adding acetic acid, and adjusting the pH value of the mixed system to 1;
weighing 1.824g of initiator APS, dissolving in 50ml of aqueous solution, transferring to a constant pressure dropping funnel, slowly dropping into the system for 60min, and reacting for 24h under the ice bath condition;
after the reaction is finished, the product is treated by ethanol and waterWashing, vacuum drying at 80 deg.C, and grinding to obtain rGO/Fe3O4the/PANI ternary nano composite material is characterized in that the feeding mass ratio of graphene oxide, ferroferric oxide and aniline is 3:7: 6;
2) preparing a water-based anticorrosive paint:
weighing 3.45g of the sanded ternary nanocomposite, wherein the solid content of the ternary nanocomposite is 13%, adding the ternary nanocomposite into water-based paint resin, stirring uniformly, and adding an amino resin curing agent to obtain the water-based nano paint, wherein the content of the nanocomposite in the coating is 3 wt%.
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