CN111303744A - Aqueous polyurethane coating containing phytic acid modified MXene and preparation method thereof - Google Patents

Aqueous polyurethane coating containing phytic acid modified MXene and preparation method thereof Download PDF

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CN111303744A
CN111303744A CN202010186128.7A CN202010186128A CN111303744A CN 111303744 A CN111303744 A CN 111303744A CN 202010186128 A CN202010186128 A CN 202010186128A CN 111303744 A CN111303744 A CN 111303744A
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phytic acid
acid modified
percent
mxene
modified mxene
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CN111303744B (en
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张力
赵炎锋
杨丽庭
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South China Normal University
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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
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
    • C08G18/625—Polymers of alpha-beta ethylenically unsaturated carboxylic acids; hydrolyzed polymers of esters of these acids
    • C08G18/6254—Polymers of alpha-beta ethylenically unsaturated carboxylic acids and of esters of these acids containing hydroxy groups
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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
    • 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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Abstract

The invention discloses a phytic acid modified MXene-containing waterborne polyurethane coating and a preparation method thereof. The phytic acid modified MXene-containing waterborne polyurethane coating is prepared from phytic acid modified MXene, acrylate monomers, functional monomers, isocyanate, an initiator, an emulsifier and water. The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps: 1) adding water into acrylate monomers, functional monomers, an initiator and an emulsifier for dispersion, and carrying out emulsion polymerization to obtain an acrylic emulsion; 2) and (3) mixing the acrylic emulsion and isocyanate, fully reacting, adding the phytic acid modified MXene, and uniformly mixing to obtain the phytic acid modified MXene-containing waterborne polyurethane coating. The phytic acid modified MXene-containing waterborne polyurethane coating disclosed by the invention is high in drying speed, non-toxic and environment-friendly, and a film formed by the coating is high in hardness and excellent in corrosion resistance.

Description

Aqueous polyurethane coating containing phytic acid modified MXene and preparation method thereof
Technical Field
The invention relates to a phytic acid modified MXene-containing waterborne polyurethane coating and a preparation method thereof, belonging to the technical field of waterborne coatings.
Background
Polyurethane (PU) coatings have the advantages of good mechanical properties, high adhesion, good corrosion resistance, etc., and have received increasing attention in the coating industry. Solvent-borne polyurethane (SPU) coatings can generate Volatile Organic Compounds (VOCs) during the coating process, which not only can pollute the environment, but also can harm the health of the constructors. The Waterborne Polyurethane (WPU) coating reduces the discharge of VOCs in the reaction process, and has the advantages of environmental protection, no toxicity, stable chemical property, no solvent smell, no pollution and the like. However, the drying time of the aqueous polyurethane coating is long, and the water resistance, oxidation resistance, corrosion resistance and other performances of a film formed by the aqueous polyurethane coating are poor, so that the aqueous polyurethane coating cannot completely replace a solvent type polyurethane coating.
Therefore, it is necessary to develop an aqueous polyurethane coating material having a film formed thereon, which has excellent oxidation resistance and excellent corrosion resistance.
Disclosure of Invention
The invention aims to provide a phytic acid modified MXene-containing waterborne polyurethane coating and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 to 10 percent;
acrylate monomer: 20 to 40 percent;
functional monomer: 5% -20%;
isocyanate: 5% -20%;
initiator: 0.01 to 0.03 percent;
emulsifier: 0.05 percent to 0.15 percent;
water: and (4) the balance.
Preferably, the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 to 1 percent;
acrylate monomer: 25 to 35 percent;
functional monomer: 7% -15%;
isocyanate: 7 to 18 percent;
initiator: 0.01 to 0.03 percent;
emulsifier: 0.05 percent to 0.15 percent;
water: and (4) the balance.
Further preferably, the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 to 0.8 percent;
acrylate monomer: 28% -34%;
functional monomer: 10% -15%;
isocyanate: 10% -15%;
initiator: 0.01 to 0.03 percent;
emulsifier: 0.05 percent to 0.15 percent;
water: and (4) the balance.
Preferably, the radial dimension of the phytic acid modified MXene is 0.05-100 μm, and the thickness of the phytic acid modified MXene is 0.5-200 nm.
Preferably, the phytic acid modified MXene is prepared by the following method: the phytic acid and MXene are mixed according to the mass ratio of (10-50): 1, mixing, performing ultrasonic dispersion, stirring at normal temperature for 0.5-48 h, centrifuging, and washing to obtain the phytic acid modified MXene.
Further preferably, the phytic acid modified MXene is prepared by the following method: the phytic acid and MXene are mixed according to the mass ratio of (15-25): 1, mixing, performing ultrasonic dispersion, stirring at normal temperature for 2-6 hours, centrifuging, and washing to obtain the phytic acid modified MXene.
Still further preferably, the phytic acid modified MXene is prepared by the following method: the phytic acid and MXene are mixed according to the mass ratio (18-22): 1, mixing, performing ultrasonic dispersion, stirring at normal temperature for 2-6 hours, centrifuging, and washing to obtain the phytic acid modified MXene.
Preferably, MXene is Ti3C2TxWherein T isxis-O, -F and-OH.
Preferably, the acrylate monomer is at least one of Methyl Acrylate (MA), Methyl Methacrylate (MMA), Ethyl Acrylate (EA), Butyl Acrylate (BA), isobornyl acrylate, and isobornyl methacrylate.
More preferably, the acrylate monomer is at least two of methyl acrylate, methyl methacrylate, ethyl acrylate and butyl acrylate.
Preferably, the functional monomer is at least one of Acrylic Acid (AA), methacrylic acid (MAA), Acrylamide (AM), hydroxypropyl acrylate (HPA), hydroxypropyl methacrylate (HPMA), Glycidyl Methacrylate (GMA), and phosphate.
Further preferably, the functional monomer is at least two of acrylic acid, methacrylic acid, acrylamide, hydroxypropyl acrylate and phosphate.
Preferably, the isocyanate is at least one of Mitsui chemical WB-3021, Mitsui chemical WD-726, Aisco G254, Aisco G265, Wanhua 268 and Wanhua 270.
More preferably, the isocyanate is at least one of estoko G254, estoko G265, wanhua 268 and wanhua 270.
Preferably, the initiator is at least one of potassium persulfate, hydrogen peroxide, sodium bisulfite, sodium thiosulfate, azobisisobutyronitrile, azobisisoheptonitrile and dibenzoyl peroxide.
More preferably, the initiator is at least one of potassium persulfate, hydrogen peroxide, sodium bisulfite, sodium thiosulfate and azobisisobutyronitrile.
Preferably, the emulsifier is at least one of dodecyl sulfonic acid betaine, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium dodecyl diphenyl ether disulfonate, isoalcohol polyoxyethylene ether ammonium sulfate, 1-allyloxy-2-hydroxypropyl sodium sulfonate and 2-acrylamide-2-methyl propyl sodium sulfonate.
More preferably, the emulsifier is at least two of dodecyl sulfonic acid betaine, dodecyl diphenyl ether disulfonic acid sodium, 1-allyloxy-2-hydroxypropyl sodium sulfonate and 2-acrylamide-2-methyl propyl sodium sulfonate.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) adding water into acrylate monomers, functional monomers, an initiator and an emulsifier for dispersion, and carrying out emulsion polymerization to obtain an acrylic emulsion;
2) and (3) mixing the acrylic emulsion and isocyanate, fully reacting, adding the phytic acid modified MXene, and uniformly mixing to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
The invention has the beneficial effects that: the phytic acid modified MXene-containing waterborne polyurethane coating disclosed by the invention is high in drying speed, non-toxic and environment-friendly, and a film formed by the coating is high in hardness and excellent in corrosion resistance.
Drawings
Fig. 1 is an XRD pattern of MXene and phytic acid modified MXene.
FIG. 2 is an infrared spectrum diagram of MXene, phytic acid and phytic acid modified MXene.
FIG. 3 is the ultraviolet absorption spectrum of MXene, phytic acid and phytic acid modified MXene.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.071 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 2:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.371 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 3:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.2 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.271 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 4:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.6 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 42.871 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 5:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 18.13 percent;
butyl acrylate: 15.8 percent;
methacrylic acid: 1.8 percent;
hydroxypropyl acrylate: 8.35 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.371 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (hydroxyl value is 1.8 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 6:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 18.13 percent;
butyl acrylate: 15.52 percent;
methacrylic acid: 3.2 percent;
hydroxypropyl acrylate: 6.67 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.931 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (hydroxyl value is 1.5 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 7:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 17.42 percent;
butyl acrylate: 12.17 percent;
methacrylic acid: 0.6 percent;
hydroxypropyl acrylate: 13.33 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.931 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.5 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 8:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 14.5 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 39.671 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Example 9:
the phytic acid modified MXene-containing waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.4 percent;
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 10.5 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.671 percent.
The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, performing ultrasonic treatment for 3min, then adding phytic acid modified MXene, performing ultrasonic treatment for 3min, and filtering by using gauze to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
Comparative example 1:
the waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
MXene：0.4％；
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.071 percent.
The preparation method of the waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, carrying out ultrasonic treatment for 3min, then adding MXene, carrying out ultrasonic treatment for 3min, and filtering by using gauze to obtain the waterborne polyurethane coating.
Comparative example 2:
the waterborne polyurethane coating is prepared from the following raw materials in percentage by mass:
methyl methacrylate: 17.47%;
butyl acrylate: 13.8 percent;
methacrylic acid: 0.9 percent;
hydroxypropyl acrylate: 12.21 percent;
phosphate ester: 0.9 percent;
wanhua 268: 11.1 percent;
potassium persulfate: 0.014%;
dodecyl sulfonic acid betaine: 0.045%;
sodium 2-acrylamido-2-methylpropanesulfonate: 0.09%;
deionized water: 43.471 percent.
The preparation method of the waterborne polyurethane coating comprises the following steps:
1) mixing 1/2 methyl methacrylate, 2/3 butyl acrylate, 1/2 methacrylic acid and 1/3 hydroxypropyl acrylate, and performing ultrasonic treatment for 5min to obtain a mixed monomer A;
2) mixing the rest methyl methacrylate, the rest butyl acrylate, the rest methacrylic acid, the rest hydroxypropyl acrylate and phosphate, and performing ultrasonic treatment for 5min to obtain a mixed monomer B;
3) uniformly mixing potassium persulfate, dodecyl sulfonic acid betaine, 2-acrylamide-2-methyl propyl sodium sulfonate and deionized water, heating to 80 ℃, dropwise adding the mixed monomer A, preserving the temperature for 30min after dropwise adding, dropwise adding the mixed monomer B, heating to 85 ℃, preserving the temperature for 1h after dropwise adding, and cooling to room temperature to obtain acrylic emulsion (the hydroxyl value is 2.1 mgKOH/g);
4) and (3) adjusting the pH value of the acrylic emulsion to 8 by using ammonia water, adding Wanhua 268, and performing ultrasonic treatment for 3min to obtain the waterborne polyurethane coating.
Note:
the phytic acid modified MXene in the embodiments 1 to 9 is prepared by the following method: mixing phytic acid and MXene according to the mass ratio of 20:1, carrying out ultrasonic reaction for 4min, stirring for 4h at normal temperature, centrifuging, washing a solid product obtained by centrifuging with deionized water until a washing liquid is neutral, and obtaining the phytic acid modified MXene (the radial dimension is 1-5 mu m, and the thickness is 2-4 nm).
MXene in examples 1 to 9 and comparative example 1 was Ti3C2TxWherein T isxis-O, -F and-OH (namely MXene contains three groups of-O, -F and-OH at the same time).
The XRD patterns of Mxene (MX) and phytic acid modified MXene (PA-MX) are shown in figure 1, the infrared spectra of MXene, Phytic Acid (PA) and phytic acid modified MXene are shown in figure 2, and the ultraviolet absorption spectra of MXene, phytic acid and phytic acid modified MXene are shown in figure 3.
As can be seen from fig. 1: after modifying MXene with phytic acid, the basal plane peak of MXene at 2 theta (6.44 degrees) is shifted to the left to 5.84 degrees which is lower, which means that the distance between PA and MXene is widened, and the modified MXene is successfully modified by PA.
As can be seen from fig. 2: at 1638cm-1Compared with pure MXene, the PA-MXene has one more absorption peak, and the PA concentration is 1640cm-1There is an absorption peak nearby, which indicates MThe Xene modification was successful.
As can be seen from fig. 3: the absorption position of P ═ O bond in the phosphoric acid group at 260nm is determined, pure MXene has no absorption here, and PA-MXene has weak absorption here, which indicates that MXene modification is successful.
And (3) performance testing:
the aqueous polyurethane coatings of examples 1-9 and comparative examples 1-2 were coated on a Q235 iron sheet and tested for performance, with the test results shown in the following table:
TABLE 1 Performance test results of the aqueous polyurethane coatings of examples 1 to 9 and comparative examples 1 to 2
Figure BDA0002414243540000121
Figure BDA0002414243540000131
Note:
surface drying time: the test is carried out according to the GB/T1727-1979 paint film general preparation method, and the specific operation is as follows: the iron sheet after polishing was coated with a film, and after the coating was completed, the sheet was dried under the drying conditions specified in the standards, and it was examined at intervals of time by a finger touch method at a distance of about 10mm from the edge of the paint film whether or not the film was dry, and if still sticky but the coating did not stick to the hand, the film was regarded as dry.
Pencil hardness: the test is carried out according to GB/T6739 + 2006 method for measuring hardness of coating pencil, and the specific operation is as follows: carrying out nib treatment on the Chinese high-grade drawing pencil with the hardness grade of 6B-6H, and grinding the nib into a sharp horizontal edge; and horizontally placing the iron sheet after being completely coated and dried on a laboratory table, holding a pencil by hand for about 35 degrees, sliding at a constant speed for about 10mm, sliding the pencil with the same mark for five times, and if only one scratch exists, determining that the hardness of the coating is the mark of the pencil.
Corrosion potential: and (3) soaking the crosslinked and cured coating in a 3.5% sodium chloride solution for about 30min, testing the OCPT, and testing the TAFEL curve after the stability is shown to be tested to obtain the corrosion current and the corrosion potential.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The phytic acid modified MXene-containing waterborne polyurethane coating is characterized by comprising the following components in parts by weight: the material is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 to 10 percent;
acrylate monomer: 20 to 40 percent;
functional monomer: 5% -20%;
isocyanate: 5% -20%;
initiator: 0.01 to 0.03 percent;
emulsifier: 0.05 percent to 0.15 percent;
water: and (4) the balance.
2. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1, wherein: the material is prepared from the following raw materials in percentage by mass:
phytic acid modified MXene: 0.1 to 1 percent;
acrylate monomer: 25 to 35 percent;
functional monomer: 7% -15%;
isocyanate: 7 to 18 percent;
initiator: 0.01 to 0.03 percent;
emulsifier: 0.05 percent to 0.15 percent;
water: and (4) the balance.
3. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1 or 2, wherein: the radial dimension of the phytic acid modified MXene is 0.05-100 μm, and the thickness is 0.5-200 nm.
4. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 3, wherein: the phytic acid modified MXene is prepared by the following method: the phytic acid and MXene are mixed according to the mass ratio of (10-50): 1, mixing, performing ultrasonic dispersion, stirring at normal temperature for 0.5-48 h, centrifuging, and washing to obtain the phytic acid modified MXene.
5. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 4, wherein: the MXene is Ti3C2TxWherein T isxis-O, -F and-OH.
6. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1 or 2, wherein: the acrylate monomer is at least one of methyl acrylate, methyl methacrylate, ethyl acrylate, butyl acrylate, isobornyl acrylate and isobornyl methacrylate.
7. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1 or 2, wherein: the functional monomer is at least one of acrylic acid, methacrylic acid, acrylamide, hydroxypropyl acrylate, hydroxypropyl methacrylate, glycidyl methacrylate and phosphate.
8. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1 or 2, wherein: the initiator is at least one of potassium persulfate, hydrogen peroxide, sodium bisulfite, sodium thiosulfate, azobisisobutyronitrile, azobisisoheptonitrile and dibenzoyl peroxide.
9. The phytic acid modified MXene-containing aqueous polyurethane coating according to claim 1 or 2, wherein: the emulsifier is at least one of dodecyl sulfonic acid betaine, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium dodecyl diphenyl ether disulfonate, isoalcohol polyoxyethylene ether ammonium sulfate, 1-allyloxy-2-hydroxypropyl sodium sulfonate and 2-acrylamide-2-methyl sodium propane sulfonate.
10. The preparation method of the phytic acid modified MXene-containing waterborne polyurethane coating as claimed in any one of claims 1 to 9, wherein the preparation method comprises the following steps: the method comprises the following steps:
1) adding water into acrylate monomers, functional monomers, an initiator and an emulsifier for dispersion, and carrying out emulsion polymerization to obtain an acrylic emulsion;
2) and (3) mixing the acrylic emulsion and isocyanate, fully reacting, adding the phytic acid modified MXene, and uniformly mixing to obtain the phytic acid modified MXene-containing waterborne polyurethane coating.
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