CN114539898B - Anticorrosive coating containing rare earth corrosion inhibitor HEDP-Ce and preparation method thereof - Google Patents
Anticorrosive coating containing rare earth corrosion inhibitor HEDP-Ce and preparation method thereof Download PDFInfo
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- CN114539898B CN114539898B CN202210208223.1A CN202210208223A CN114539898B CN 114539898 B CN114539898 B CN 114539898B CN 202210208223 A CN202210208223 A CN 202210208223A CN 114539898 B CN114539898 B CN 114539898B
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- 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
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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
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Abstract
The invention discloses a preparation method of an anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce, which comprises the following steps: step 1, preparing a rare earth corrosion inhibitor HEDP-Ce; step 2, sequentially adding polyol resin and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine, adding HEDP-Ce after stirring at the initial rotating speed, resetting the rotating speed of the dispersion machine, continuing dispersion, replacing the dispersion disc with a grinding disc after dispersion is finished, adding zirconium beads for grinding, testing the particle size of HEDP-Ce, stopping grinding when the particle size of HEDP-Ce is not more than 15um, filtering the zirconium beads, sequentially adding a leveling agent, a wetting dispersant and a curing agent, and uniformly dispersing to obtain the polyurethane anticorrosive paint; and 3, uniformly coating the polyurethane anticorrosive paint obtained in the step 2 on the surface of the base material by using a four-side coater to obtain the polyurethane anticorrosive paint. The method solves the problem of poor corrosion resistance of the existing polyurethane coating.
Description
Technical Field
The invention belongs to the technical field of anticorrosive coatings, and relates to an anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce, and a preparation method of the anticorrosive coating containing the rare earth corrosion inhibitor HEDP-Ce.
Background
The corrosion and protection are always important links of industrial production, and the investment in corrosion protection in the whole economy every year is huge. In order to reduce the risk of corrosion or to retard the progress of corrosion, the surfaces susceptible to corrosion are often protected by various methods, particularly using current coating techniques. Among them, the addition of corrosion inhibitors to organic coatings is a versatile and efficient method. The organic corrosion inhibitor usually contains heteroatom N, O, S, lone pair electrons of which coordinate with empty orbitals of metal to form a layer of protective film which is adsorbed on the surface of a base material so as to achieve good corrosion prevention effect. However, the organic corrosion inhibitor has a single effect, and is often compounded with some inorganic corrosion inhibitors, and the organic corrosion inhibitor and the inorganic corrosion inhibitors can achieve a synergistic effect, so that the corrosion inhibition efficiency is greatly improved. The preparation of the novel corrosion inhibitor provides a new idea for improving the anti-corrosion performance of the polyurethane coating. In the invention, the novel material HEDP-Ce is successfully prepared, and after the compound is purified, the compound is utilized and then is ground and dispersed in a polyurethane organic coating to obtain the coating material. By coating easily-corroded materials such as steel, a better protection effect is generated compared with a polyurethane coating without the corrosion inhibition material as a reference material.
Disclosure of Invention
The invention aims to provide a preparation method of an anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce, which solves the problem of poor anticorrosive performance of the existing polyurethane coating.
Another object of the invention is to provide an anticorrosive coating containing the rare earth corrosion inhibitor HEDP-Ce.
The technical scheme adopted by the invention is that the preparation method of the anticorrosive coating of the rare earth corrosion inhibitor HEDP-Ce is implemented according to the following steps:
step 1, preparing a rare earth corrosion inhibitor HEDP-Ce;
step 2, sequentially adding polyol resin and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine, stirring at the initial rotating speed, adding HEDP-Ce obtained in the step 1, resetting the rotating speed of the dispersion machine, continuously dispersing, replacing the dispersion disk with a grinding disk after dispersion is finished, adding zirconium beads for grinding, testing the particle size of HEDP-Ce in the grinding process, stopping grinding until the particle size of HEDP-Ce is not more than 15 mu m, filtering the zirconium beads, sequentially adding a leveling agent, a wetting dispersant and a curing agent, and uniformly dispersing to obtain the polyurethane anticorrosive paint;
and 3, uniformly coating the polyurethane anticorrosive paint obtained in the step 2 on the surface of the base material by using a four-side coater, and curing at room temperature to obtain the polyurethane anticorrosive paint.
The present invention is also characterized in that,
the specific process of the step 1 is as follows: adding Ce (NO) 3 ) 3 ·6H 2 And dropwise adding the O solution into HEDP, stirring at room temperature until the solution becomes a white turbid solution, standing to enable the complex to be fully precipitated, filtering by using a sand core funnel to obtain a white substance, washing the white substance by using ethanol for 3-4 times, drying in a vacuum oven, pouring into a mortar after drying, and grinding to obtain white powder to obtain the rare earth corrosion inhibitor HEDP-Ce.
Ce(NO 3 ) 3 ·6H 2 The molar ratio of O to HEDP is 1:1; ce (NO) 3 ) 3 ·6H 2 Water and Ce (NO) in O solution 3 ) 3 ·6H 2 The mass ratio of O is 100.
In the step 2, the mass ratio of the polyol resin, the butyl acetate, the HEDP-Ce, the flatting agent, the wetting dispersant and the curing agent is 30:7.295:0 to 0.42:1:1:11.79.
in step 2, the initial rotating speed is 1000r/min, the stirring time is 10min, the reset rotating speed is 1200r/min, the continuous dispersion time is 20min, and the rotating speed during grinding is 1500r/min.
In the step 2, the mass of the zirconium beads is 1.6 times of the sum of the mass of the polyol resin and the mass of the butyl acetate.
In the step 3, the thickness of the wet film is 100 +/-10 mu m, and the thickness of the dry film of the polyurethane anticorrosive coating after 7 days of curing is 35 +/-5 mu m.
The other technical scheme adopted by the invention is that the anticorrosive coating of the rare earth corrosion inhibitor HEDP-Ce is prepared by the preparation method.
The invention has the beneficial effects that compared with the coating without the rare earth corrosion inhibitor, the anticorrosive coating containing the rare earth corrosion inhibitor HEDP-Ce has higher hardness, better toughness and higher corrosion resistance, and the corrosion resistance of the obtained polyurethane anticorrosive coating is greatly improved by adding the rare earth corrosion inhibitor HEDP-Ce.
Drawings
FIG. 1 is a corrosion resistance test result of an embodiment of the preparation method of the anticorrosive coating of the rare earth corrosion inhibitor HEDP-Ce of the invention; (a) is the test result of example 1, (b) is the test result of example 2, (c) is the test result of example 3, and (d) is the test result of example 4;
FIG. 2 is an XRD spectrum of the rare earth corrosion inhibitor HEDP-Ce of the invention;
FIG. 3 is an EDS spectrum of the rare earth corrosion inhibitor HEDP-Ce of the invention.
FIG. 4 is a schematic illustration of the rare earth corrosion inhibitor HEDP-Ce to extend the penetration of corrosive media.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of an anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce, which is implemented according to the following steps:
step 1, preparing a rare earth corrosion inhibitor HEDP-Ce, which comprises the following specific steps:
first, ce (NO) is prepared 3 ) 3 ·6H 2 O solution, ce (NO) 3 ) 3 ·6H 2 Water and Ce (NO) in O solution 3 ) 3 ·6H 2 The mass ratio of O is 100;
adding Ce (NO) 3 ) 3 ·6H 2 And dropwise adding the O solution into HEDP, stirring to obtain a white turbid solution, reacting at room temperature for 2 hours, and standing for 12 hours to fully precipitate the complex. Filtering with a sand core funnel to obtain a white substance, washing the white substance with ethanol for 3-4 times, putting the white substance into a vacuum oven at the temperature of 70 ℃ for drying for 12h, pouring the white substance into a mortar after drying, and grinding the white substance into white powder to obtain a rare earth corrosion inhibitor HEDP-Ce;
Ce(NO 3 ) 3 ·6H 2 the molar ratio of O to HEDP is 1:1;
the reaction equation is as follows:
description of the drawings: the position of H on phosphonic acid is not exclusive and is a possible structure for charge conservation.
Step 2, sequentially adding a polyol resin (73864, solid content of 70%) and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine to be 1000r/min, stirring for 10min at the initial rotating speed, adding HEDP-Ce (based on 0wt%, 0.5wt%, 1.0wt% and 2.0wt% of the solid content of the polyol resin) obtained in the step 1, resetting the rotating speed of the dispersion machine to be 1200r/min, continuously dispersing for 20min, replacing the dispersion disc with a grinding disc after dispersion is finished, adding zirconium beads for grinding, testing the particle size of HEDP-Ce during grinding, stopping grinding until the particle size of HEDP-Ce is not more than 15um, sequentially adding a leveling agent, filtering, wetting a dispersing agent and a curing agent, and uniformly dispersing to obtain the polyurethane anticorrosive paint;
the mass ratio of the polyol resin, the butyl acetate, the HEDP-Ce, the flatting agent, the wetting dispersant and the curing agent is 30:7.295:0 to 0.42:1:1:11.79;
the mass of the zirconium beads is 1.6 times of the sum of the mass of the polyol resin and the mass of the butyl acetate;
and 3, uniformly coating the polyurethane anticorrosive coating obtained in the step 2 on the surface of a base material by using a four-side coater, wherein the thickness of a wet film is 100 +/-10 microns, and after curing for 7 days at room temperature, the thickness of a dry film of the polyurethane anticorrosive coating is 35 +/-5 microns.
The invention selects the hydroxyl ethylidene diphosphonic acid (HEDP) as the organic corrosion inhibitor and the Ce (NO) as the inorganic corrosion inhibitor 3 ) 3 ·6H 2 And O compounding to prepare a functional material HEDP-Ce with corrosion inhibition performance, and adding the functional material HEDP-Ce into the polyurethane coating. HEDP molecules have high-polarity P-O bonds, and hydroxyl (-OH) exists in the molecules, and the hydroxyl can react with isocyanate, so that the corrosion inhibitor molecules directly participate in the construction of a cross-linked network and promote the curing of a polyurethane coating; oxygen (O) and Ce (NO) in the molecule 3 ) 3 Ce in (1) 3+ Has strong coordination ability; different from the prior corrosion inhibitor, the HEDP-Ce corrosion inhibitor particles prepared by the invention have double protection effects on the base material: (1) Wherein HEDP has strong chelating effect and can chelate Fe 2+ Chelate is formed at the coating defect, the reaction activity of the anode is reduced, and the dissolution of iron is inhibited; (2) Ce 3+ The presence of ions may also interact with traces of OH in the environment - Forming an insoluble protective film on the cathode; in addition, HEDP-Ce can also be used as a filler to extend corrosive mediaThe path of the penetration further improves the corrosion protection of the polyurethane coating, as shown in fig. 4.
Example 1
Step 1, sequentially adding polyol resin (73864, solid content of 70%) and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine to be 1000r/min, stirring for 10min at the initial rotating speed, resetting the rotating speed of the dispersion machine to be 1200r/min, continuing to disperse for 20min, sequentially adding a leveling agent, a wetting dispersant and a curing agent (hexamethylene diisocyanate type isocyanate (N3390)) after the dispersion is finished, and uniformly dispersing to obtain the polyurethane anticorrosive paint;
and 2, uniformly coating the polyurethane anticorrosive coating obtained in the step 1 on the surface of a base material by using a four-side coater, wherein the thickness of a wet film is 100 +/-10 microns, and after curing for 7 days at room temperature, the thickness of a dry film of the polyurethane anticorrosive coating is 35 +/-5 microns.
Example 2
Step 1, preparing a rare earth corrosion inhibitor HEDP-Ce, which comprises the following specific steps:
first Ce (NO) 3 ) 3 ·6H 2 O solution, ce (NO) 3 ) 3 ·6H 2 Water and Ce (NO) in O solution 3 ) 3 ·6H 2 The mass ratio of O is 100;
ce (NO) 3 ) 3 ·6H 2 And dropwise adding the O solution into HEDP, stirring to obtain a white turbid solution, reacting at room temperature for 2 hours, and standing for 12 hours to fully precipitate the complex. Filtering with a sand core funnel to obtain a white substance, washing the white substance with ethanol for 3-4 times, putting the white substance into a vacuum oven at the temperature of 70 ℃ for drying for 12h, pouring the white substance into a mortar after drying, and grinding the white substance into white powder to obtain a rare earth corrosion inhibitor HEDP-Ce;
Ce(NO 3 ) 3 ·6H 2 the molar ratio of O to HEDP is 1:1;
step 2, sequentially adding polyol resin (73864, solid content of 70%) and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine to be 1000r/min, stirring for 10min at the initial rotating speed, adding HEDP-Ce (based on 0.5wt% of the solid content of the polyol resin) obtained in the step 1, resetting the rotating speed of the dispersion machine to be 1200r/min, continuing to disperse for 20min, replacing the dispersion disc with a grinding disc after dispersion is finished, adding zirconium beads for grinding, wherein the rotating speed during grinding is 1500r/min, testing the particle size of HEDP-Ce in the grinding process, stopping grinding until the particle size of HEDP-Ce is not more than 15um, filtering out the zirconium beads, sequentially adding a leveling agent, a wetting dispersant and a curing agent (hexamethylene diisocyanate type isocyanate (N3390)), and uniformly dispersing to obtain the polyurethane anticorrosive paint;
the mass of the zirconium beads is 1.6 times of the sum of the mass of the polyol resin and the mass of the butyl acetate;
and 3, uniformly coating the polyurethane anticorrosive coating obtained in the step 2 on the surface of a base material by using a four-side coater, wherein the thickness of a wet film is 100 +/-10 microns, and after curing for 7 days at room temperature, the thickness of a dry film of the polyurethane anticorrosive coating is 35 +/-5 microns.
Example 3
The difference from example 2 is that: the addition amount of HEDP-Ce is as follows: 1wt% based on the amount of polyol resin solids;
example 4
The difference from example 2 is that: the addition amount of HEDP-Ce is as follows: based on 2wt% of the polyol resin solids. The amounts of each raw material added in examples 1 to 4 are shown in table 1:
TABLE 1 raw material addition amount
| Components | Example 1 | Example 2 | Example 3 | Example 4 |
| Polyhydric alcoholsResin (g) | 60.00 | 60.00 | 60.00 | 60.00 |
| Butyl acetate (g) | 14.59 | 14.59 | 14.59 | 14.59 |
| HEDP-Ce(g) | 0.00 | 0.21 | 0.42 | 0.84 |
| Flatting agent (g) | 2.00 | 2.00 | 2.00 | 2.00 |
| Wetting dispersant (g) | 2.00 | 2.00 | 2.00 | 2.00 |
| Curing agent (g) | 23.58 | 23.58 | 23.58 | 23.58 |
FIGS. 1 (a), (b), (c) and (d) are the results of the experiments of example 1, example 2, example 3 and example 4 after the salt spray box is exposed for 144h, respectively, and the corrosion resistance of the coating can be observed from the corrosion at and around the scratch; as is apparent from the figure, the coating of example 1 without adding the HEDP-Ce corrosion inhibitor has bubbling at the scratch, and the black corrosion products around the scratch are particularly obviously accumulated, the surface corrosion is the most severe, and the corrosion resistance of the coating is the worst; the accumulation of corrosion products near the scratches of the coatings of examples 2, 3 and 4 is greatly reduced, and the corrosion at the scratches tends to be weakened; the results of the experiment show that the effect of the example 1 is the worst, and in conclusion, the following conclusion can be drawn: the corrosion resistance of the polyurethane coating can be enhanced by adding the corrosion inhibitor particles HEDP-Ce.
As can be seen from FIG. 2, the XRD pattern of the product HEDP-Ce and Ce (NO) 3 ) 3 ·6H 2 The O and HEDP comparisons are quite different and thus indicate a new compound. As can be seen from the spectrum of FIG. 3, the presence of Ce is evident in the graph, which proves the success of HEDP-Ce preparation.
Claims (2)
1. A preparation method of an anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce is characterized by comprising the following steps:
step 1, preparing a rare earth corrosion inhibitor HEDP-Ce;
the specific process of the step 1 is as follows: ce (NO) 3 ) 3 ·6H 2 Dropwise adding the O solution into HEDP, stirring until the solution becomes a white turbid solution, standing to enable the complex to be fully precipitated, filtering by using a sand core funnel to obtain a white substance, washing the white substance by using ethanol for 3-4 times, putting the white substance into a vacuum oven for drying, pouring the white substance into a mortar after drying, and grinding the white substance into white powder to obtain a rare earth corrosion inhibitor HEDP-Ce;
Ce(NO 3 ) 3 ·6H 2 the molar ratio of O to HEDP was 1:1; ce (NO) 3 ) 3 ·6H 2 Water and Ce (NO) in O solution 3 ) 3 ·6H 2 The mass ratio of O is 100;
step 2, sequentially adding polyol resin and butyl acetate into a grinding tank, setting the initial rotating speed of a dispersion machine, stirring at the initial rotating speed, adding HEDP-Ce obtained in the step 1, resetting the rotating speed of the dispersion machine, continuously dispersing, replacing the dispersion disk with a grinding disk after dispersion is finished, adding zirconium beads for grinding, testing the particle size of HEDP-Ce in the grinding process, stopping grinding until the particle size of HEDP-Ce is not more than 15 mu m, filtering the zirconium beads, sequentially adding a leveling agent, a wetting dispersant and a curing agent, and uniformly dispersing to obtain the polyurethane anticorrosive paint;
the mass ratio of the polyol resin, the butyl acetate, the HEDP-Ce, the flatting agent, the wetting dispersant and the curing agent is 30:7.295:0 to 0.42:1:1:11.79;
the initial rotating speed is 1000r/min, the stirring time is 10min, the reset rotating speed is 1200r/min, the continuous dispersion time is 20min, and the rotating speed during grinding is 1500r/min;
the mass of the zirconium beads is 1.6 times of the sum of the mass of the polyol resin and the mass of the butyl acetate;
step 3, uniformly coating the polyurethane anticorrosive paint obtained in the step 2 on the surface of a base material by using a four-side coater, and curing at room temperature to obtain a polyurethane anticorrosive coating;
the thickness of the wet film is 100 +/-10 mu m, and the dry film thickness of the polyurethane anti-corrosion coating is 35 +/-5 mu m after curing for 7 days.
2. An anticorrosive coating containing a rare earth corrosion inhibitor HEDP-Ce, which is characterized by being prepared by the preparation method of claim 1.
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| EP1726688A1 (en) * | 2005-05-23 | 2006-11-29 | Shin-Etsu Chemical Co., Ltd. | Cerium ion-containing solution and corrosion inhibitor |
| CN105177561A (en) * | 2015-08-21 | 2015-12-23 | 山东大学 | Aluminum or aluminum alloy protection chromium-free passivation solution, preparation method and aluminum or aluminum alloy surface protection method thereof |
| CN110760854A (en) * | 2018-07-26 | 2020-02-07 | 天津大学 | Hydroxyethylidene diphosphonic acid intercalated zinc-aluminum hydrotalcite corrosion inhibitor and preparation method thereof |
| EP3663435B1 (en) * | 2018-12-05 | 2024-03-13 | Henkel AG & Co. KGaA | Passivation composition based on mixtures of phosphoric and phosphonic acids |
| CN110819149B (en) * | 2019-12-13 | 2021-09-24 | 南昌航空大学 | Preparation method of fibrous rare earth antirust pigment |
| CN111453862B (en) * | 2020-04-09 | 2023-01-06 | 成都纺织高等专科学校 | Multi-component compound corrosion inhibitor for magnesium and magnesium alloy and application method thereof |
| CN113698859A (en) * | 2021-07-22 | 2021-11-26 | 成都普瑞斯特新材料有限公司 | High-weather-resistance polyurethane anticorrosive paint and preparation method thereof |
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