CN113249024A - Preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane - Google Patents
Preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane Download PDFInfo
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- CN113249024A CN113249024A CN202110666256.6A CN202110666256A CN113249024A CN 113249024 A CN113249024 A CN 113249024A CN 202110666256 A CN202110666256 A CN 202110666256A CN 113249024 A CN113249024 A CN 113249024A
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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
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- 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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Abstract
The invention discloses a preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane, which comprises the steps of preparing cerium ion modified montmorillonite, preparing tannic acid modified cerium ion modified montmorillonite, and preparing tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane anticorrosive paint. In the tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane coating, tannic acid and cerium ions as corrosion inhibitors can react with corrosion products to generate insoluble substances to block corrosion processes, and montmorillonite plays a role in physical barrier and blocks penetration of corrosion media, so that the coating has good water resistance and corrosion resistance, and the preparation method is simple and environment-friendly, and has a wide application prospect in the field of anticorrosive coatings.
Description
Technical Field
The invention relates to the technical field of anticorrosive coatings, in particular to a preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane.
Background
Corrosion of metal materials causes great economic loss and safety problems, and thus it is essential to protect the metal materials from corrosion. Surface coatings are the most common and effective corrosion protection techniques, wherein solvent-based coatings are limited in their application due to their toxicity and fouling properties due to the large amount of organic solvents contained; the water-based paint has the advantages of no toxicity, no pollution, energy conservation and the like, but the water resistance, the thermal stability and the corrosion resistance of the water-based paint are generally poor.
At present, many researches on improving the corrosion resistance of the waterborne polyurethane coating are carried out, and certain research results are obtained. Patent application No. 202010091012.5 provides a functionalized graphene waterborne polyurethane anticorrosive paint and a preparation method thereof. An aqueous fluorocarbon modified acrylic polyurethane coating is provided in patent application No. 202010696772.9. Patent application No. 201911243457.4 provides a two-component water-based anticorrosive coating based on a fluorine polyimide modified curing agent. Although the corrosion resistance of the coating is improved to some extent, there is nevertheless a clear gap compared to solvent-based coatings.
The montmorillonite is a natural two-dimensional nano material, the thickness of a single montmorillonite layer is only about 1nm, and a labyrinth effect can be formed in the coating by adding a small amount of montmorillonite in the aqueous polyurethane coating, so that the diffusion path of a corrosive medium is effectively increased, and the corrosion resistance of the coating is improved. However, poor water absorption of the filler and poor dispersibility in the coating can reduce the corrosion protection properties of the aqueous polyurethane coating.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane anticorrosive paint.
The purpose of the invention is realized by the following technical scheme: a preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane comprises the following steps:
s1, preparing cerium ion modified montmorillonite;
adding sodium-based montmorillonite into deionized water, stirring to obtain a suspension, adding cerium nitrate, heating and stirring, centrifuging, drying and grinding to obtain cerium ion modified montmorillonite;
s2, preparing tannin modified cerium ion modified montmorillonite;
adding the cerium ion modified montmorillonite prepared in the step S1 into deionized water, stirring to obtain a suspension, adding tannic acid, adjusting the pH value of the suspension, continuing stirring for reaction, and then centrifuging, drying and grinding to obtain the tannic acid modified cerium ion modified montmorillonite;
s3, preparing tannin modified cerium ion modified montmorillonite/waterborne polyurethane;
heating and stirring polyol, polyisocyanate, a catalyst and a chain extender-1 for reaction, adding a chain extender-2 for continuous reaction, cooling and adding a salt forming agent, dispersing the tannin modified cerium particle modified montmorillonite obtained in the step S2 in deionized water, slowly adding the montmorillonite and stirring at a high speed, and emulsifying to obtain the tannin modified cerium ion modified montmorillonite/waterborne polyurethane.
Preferably, in the S2, the suspension has a pH of 8.0 to 8.5.
Preferably, in S3, the polyol is PPG 2000, the polyisocyanate is TPDI, the catalyst is DBTDL, the chain extender-1 is DMPA, the chain extender-2 is BDO, and the salt former is TEA.
Preferably, in said S3, the molar ratio of-NCO groups to-OH groups is 1.3: 1.
Preferably, in S3, the tannic acid-modified cerium ion-modified montmorillonite accounts for 0.5 to 2% by mass of the aqueous polyurethane resin.
The room temperature and the unspecified temperature are both 20-30 ℃.
The invention has the beneficial effects that:
1. and replacing sodium ions among montmorillonite layers with cerium ions through ion exchange reaction to prepare the cerium ion modified montmorillonite. The cerium ions as the corrosion inhibitor can react with OH < - > generated by the cathode to generate insoluble substances to be deposited on a corrosion part, thereby effectively blocking the corrosion process. The physical barrier effect of the montmorillonite improves the permeability resistance of the coating.
2. Preparing the tannic acid modified cerium ion modified montmorillonite. The addition of tannic acid improves the dispersibility of the filler in the resin, and simultaneously, the tannic acid is an effective anode inhibitor and reacts with iron ions to form a difficultly soluble TA-Fe3+ complex.
3. Preparing the tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane anticorrosive paint. Compared with the single use of montmorillonite, the tannin modified cerium ion modified montmorillonite nanosheet material can provide better corrosion protection performance for the waterborne polyurethane coating.
Drawings
FIG. 1 is a scanning electron micrograph of tannic acid modified cerium ion modified montmorillonite;
FIG. 2 is comparative EIS test patterns of several waterborne polyurethanes.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following.
Example 1
The embodiment relates to a preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane, which comprises the following steps:
1) preparing cerium ion modified montmorillonite: weighing 1g of Na-MMT (sodium montmorillonite), immersing the Na-MMT (sodium montmorillonite) in 100mL of deionized water, stirring for 2H at room temperature, adding 5.5g of Ce (NO3) 3.6H 2O (cerium nitrate) into the suspension, stirring for 24H at 80 ℃, cooling the suspension to room temperature, centrifuging for 5 times (5000r, 5min), placing in an oven, drying for 12-14H at 80 ℃, and grinding to obtain cerium ion modified montmorillonite;
2) preparing tannin modified cerium ion modified montmorillonite: weighing 0.5g of the cerium ion modified montmorillonite obtained in the step 1), adding 50mL of deionized water, stirring for 4h to obtain a stable suspension, adding 1g of tannic acid, adjusting the pH of the suspension to 8-8.5 by using tris (hydroxymethyl) aminomethane, stirring for 6h at room temperature, centrifuging the obtained product for 5 times (5000r, 5min), placing the product in an oven, drying for 12-14 h at 80 ℃, and grinding to obtain the tannic acid modified cerium ion modified montmorillonite;
3) preparing a tannin modified cerium ion modified montmorillonite/waterborne polyurethane coating and a coating: PPG 2000 and DMPA were placed in a vacuum oven at 120 ℃ in advance to remove water. 24.75g of PPG 2000, 20.25g of IPDI, 2.68g of DMPA and 4 drops of DBTDL are poured into a three-neck flask, stirred and reacted for 3h at 80 ℃, the temperature is reduced to 70 ℃, 3.92g of BDO is added, stirred and reacted for 4h, the temperature is reduced to 35 ℃, 2.02g of triethylamine is added, and the reaction is carried out for 0.5h, so that a substance a is obtained. Weighing 0.1g of the tannic acid modified cerium ion modified montmorillonite prepared in the step 2), adding 46g of deionized water, and fully stirring to obtain a stable suspension. And (3) installing a stirrer, weighing 20g of the prepared substance a, pouring into a 500mL beaker, slowly adding the aqueous dispersion containing the tannic acid modified cerium ion modified montmorillonite, stirring at a high speed (the rotating speed is 1000r/min, and the time is 45min), and emulsifying to obtain the tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane. And (3) uniformly coating the coating on the surface of the Q235 steel sheet, and sequentially placing the steel sheet at room temperature for 2d and 50 ℃ for 24h to obtain the coating.
Example 2
The embodiment relates to a preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane, which comprises the following steps:
1) preparing cerium ion modified montmorillonite: weighing 1g of Na-MMT (sodium montmorillonite), immersing the Na-MMT (sodium montmorillonite) in 100mL of deionized water, stirring for 2H at room temperature, adding 5.5g of Ce (NO3) 3.6H 2O (cerium nitrate) into the suspension, stirring for 24H at 80 ℃, cooling the suspension to room temperature, centrifuging for 5 times (5000r, 5min), placing in an oven, drying for 12-14H at 80 ℃, and grinding to obtain cerium ion modified montmorillonite;
2) preparing tannin modified cerium ion modified montmorillonite: weighing 0.5g of the cerium ion modified montmorillonite obtained in the step 1), adding 50mL of deionized water, stirring for 4h to obtain a stable suspension, adding 1g of tannic acid, adjusting the pH of the suspension to 8-8.5 by using tris (hydroxymethyl) aminomethane, stirring for 6h at room temperature, centrifuging the obtained product for 5 times (5000r, 5min), placing the product in an oven, drying for 12-14 h at 80 ℃, and grinding to obtain the tannic acid modified cerium ion modified montmorillonite;
3) preparing a tannin modified cerium ion modified montmorillonite/waterborne polyurethane coating and a coating: PPG 2000 and DMPA were placed in a vacuum oven at 120 ℃ in advance to remove water. 24.75g of PPG 2000, 20.25g of IPDI, 2.68g of DMPA and 4 drops of DBTDL are poured into a three-neck flask, stirred and reacted for 3h at 80 ℃, the temperature is reduced to 70 ℃, 3.92g of BDO is added, stirred and reacted for 4h, the temperature is reduced to 35 ℃, 2.02g of triethylamine is added, and the reaction is carried out for 0.5h, so that a substance a is obtained. Weighing 0.2g of the tannic acid modified cerium ion modified montmorillonite prepared in the step 2), adding 46g of deionized water, and fully stirring to obtain a stable suspension. And (3) installing a stirrer, weighing 20g of the prepared substance a, pouring into a 500mL beaker, slowly adding the aqueous dispersion containing the tannic acid modified cerium ion modified montmorillonite, stirring at a high speed (the rotating speed is 1000r/min, and the time is 45min), and emulsifying to obtain the tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane. And (3) uniformly coating the coating on the surface of the Q235 steel sheet, and sequentially placing the steel sheet at room temperature for 2d and 50 ℃ for 24h to obtain the coating.
Comparative example 1
Preparation of cerium ion modified montmorillonite/waterborne polyurethane
PPG 2000 and DMPA were placed in a vacuum oven at 120 ℃ in advance to remove water. 24.75g of PPG 2000, 20.25g of IPDI, 2.68g of DMPA and 4 drops of DBTDL are poured into a three-neck flask, stirred and reacted for 3h at 80 ℃, the temperature is reduced to 70 ℃, 3.92g of BDO is added, stirred and reacted for 4h, the temperature is reduced to 35 ℃, 2.02g of triethylamine is added, and the reaction is carried out for 0.5h, so that a substance a is obtained. 0.1g of cerium ion modified montmorillonite is weighed, 46g of deionized water is added, and the mixture is fully stirred to obtain stable suspension. And (3) installing a stirrer, weighing 20g of the prepared substance a, pouring into a 500mL beaker, slowly adding the aqueous dispersion containing the cerium ion modified montmorillonite, stirring at a high speed (the rotating speed is 1000r/min, and the time is 45min), and emulsifying to obtain the cerium ion modified montmorillonite/waterborne polyurethane. And uniformly coating the coating on the surface of a Q235 steel sheet, and sequentially placing the steel sheet at room temperature for 2d and 50 ℃ for 24 h.
Comparative example 2
Preparation of unmodified MMT/waterborne polyurethane
PPG 2000 and DMPA were placed in a vacuum oven at 120 ℃ in advance to remove water. 24.75g of PPG 2000, 20.25g of IPDI, 2.68g of DMPA and 4 drops of DBTDL are poured into a three-neck flask, stirred and reacted for 3h at 80 ℃, the temperature is reduced to 70 ℃, 3.92g of BDO is added, stirred and reacted for 4h, the temperature is reduced to 35 ℃, 2.02g of triethylamine is added, and the reaction is carried out for 0.5h, so that a substance a is obtained. 0.1g of Na-MMT (sodium montmorillonite) is weighed, 46g of deionized water is added, and the mixture is fully stirred to obtain a stable suspension. And (3) installing a stirrer, weighing 20g of the prepared substance a, pouring into a 500mL beaker, slowly adding the aqueous dispersion containing the sodium montmorillonite into the beaker, stirring at a high speed (the rotating speed is 1000r/min, and the time is 45min), and emulsifying to obtain the unmodified MMT/waterborne polyurethane. And uniformly coating the coating on the surface of a Q235 steel sheet, and sequentially placing the steel sheet at room temperature for 2d and 50 ℃ for 24 h.
As shown in FIG. 1, which is a scanning electron micrograph of montmorillonite modified by cerium ions modified by tannic acid, it can be seen that the modified montmorillonite has an irregular sheet structure and a rough surface.
EIS test was carried out after the tannic acid modified cerium ion montmorillonite/aqueous polyurethane anticorrosive coatings obtained in examples 1 and 2 of the present invention and comparative examples 1 and 2 were immersed in the same salt solution for 55 days, and the results are shown in FIG. 2 (examples 1 and 2 correspond to diagrams (a) and (b), respectively; comparative examples 1 and 2 correspond to diagrams (c) and (d), respectively). As can be seen from the figure, the corrosion resistance of the tannin modified cerium ion modified montmorillonite/waterborne polyurethane anticorrosive paint obtained in the examples 1 and 2 is stronger than that of the comparative examples 1 and 2.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing cerium ion modified montmorillonite;
adding sodium-based montmorillonite into deionized water, stirring to obtain a suspension, adding cerium nitrate, heating and stirring, centrifuging, drying and grinding to obtain cerium ion modified montmorillonite;
s2, preparing tannin modified cerium ion modified montmorillonite;
adding the cerium ion modified montmorillonite prepared in the step S1 into deionized water, stirring to obtain a suspension, adding tannic acid, adjusting the pH value of the suspension, continuing stirring for reaction, and then centrifuging, drying and grinding to obtain the tannic acid modified cerium ion modified montmorillonite;
s3, preparing tannin modified cerium ion modified montmorillonite/waterborne polyurethane;
heating and stirring polyol, polyisocyanate, a catalyst and a chain extender-1 for reaction, adding a chain extender-2 for continuous reaction, cooling and adding a salt forming agent, dispersing the tannic acid modified cerium ion modified montmorillonite obtained in the step S2 in deionized water, slowly adding the tannic acid modified cerium ion modified montmorillonite and stirring at a high speed, and emulsifying to obtain the tannic acid modified cerium ion modified montmorillonite/waterborne polyurethane.
2. The method for preparing the tannin modified cerium ion modified montmorillonite/waterborne polyurethane as claimed in claim 1, wherein the method comprises the following steps: in the S2, the pH value of the suspension is 8.0-8.5.
3. The method for preparing the tannin modified cerium ion modified montmorillonite/waterborne polyurethane as claimed in claim 1, wherein the method comprises the following steps: in the S3, the polyalcohol is PPG 2000, the polyisocyanate is TPDI, the catalyst is DBTDL, the chain extender-1 is DMPA, the chain extender-2 is BDO, and the salt forming agent is TEA.
4. The method for preparing the tannin modified cerium ion modified montmorillonite/waterborne polyurethane as claimed in claim 1, wherein the method comprises the following steps: in said S3, the molar ratio of-NCO groups to-OH groups is 1.3: 1.
5. The method for preparing the tannin modified cerium ion modified montmorillonite/waterborne polyurethane as claimed in claim 1, wherein the method comprises the following steps: in the S3, the tannin modified cerium ion modified montmorillonite accounts for 0.5-2% of the mass of the aqueous polyurethane resin.
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Cited By (5)
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| CN113788989A (en) * | 2021-09-13 | 2021-12-14 | 桂林理工大学 | Starch-based nano composite material with ultraviolet shielding function and preparation method thereof |
| CN115449273A (en) * | 2022-10-23 | 2022-12-09 | 青岛海洋新材料科技有限公司 | Modified anticorrosive paint and preparation method and application thereof |
| CN115851092A (en) * | 2022-12-12 | 2023-03-28 | 福州大学 | Preparation method of modified mica flake-polyurethane composite water-based paint |
| CN116479653A (en) * | 2023-04-10 | 2023-07-25 | 浙江加佳领带服装有限公司 | Softening treatment process for clothing fabric |
| CN117504439A (en) * | 2023-12-11 | 2024-02-06 | 安庆师范大学 | Denitration catalytic filter material based on tannic acid modification and preparation method and application thereof |
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| CN117504439A (en) * | 2023-12-11 | 2024-02-06 | 安庆师范大学 | Denitration catalytic filter material based on tannic acid modification and preparation method and application thereof |
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Application publication date: 20210813 |