CN111471389A - Silicon dioxide microcapsule self-repairing anticorrosive coating and preparation method thereof - Google Patents
Silicon dioxide microcapsule self-repairing anticorrosive coating and preparation method thereof Download PDFInfo
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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
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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
- 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 provides a silicon dioxide microcapsule self-repairing anticorrosive coating and a preparation method thereof, wherein the self-repairing anticorrosive coating is prepared by dispersing an oil phase formed by a corrosion inhibitor and ether in a water phase formed by ammonia water, an emulsifier and water, then dropwise adding tetraethoxyethyl orthosilicic acid to react to obtain an emulsion, then aging, washing and drying to obtain a self-repairing microcapsule material, and then uniformly stirring the microcapsule material, a polyurethane emulsion, an acrylic emulsion, a filler, a defoaming agent and a thixotropic agent. The microcapsule material formed by the silicon dioxide coated corrosion inhibitor is added into the self-repairing anticorrosive coating provided by the invention, and the corrosion inhibitor has good fluidity, high activity and good stability, so that the self-repairing efficiency of the coating is improved, the service life is effectively prolonged, and the used material has the advantages of low price, simple process, low preparation cost and wide application prospect.
Description
Technical Field
The invention relates to the technical field of anticorrosive coatings, in particular to a silicon dioxide microcapsule self-repairing anticorrosive coating and a preparation method thereof.
Background
The anticorrosive paint is a paint widely applied in modern industry, traffic, energy, ocean engineering and other departments, and the anticorrosive paint refers to a liquid or solid material which can form a film to protect, decorate or have other special functions when being coated on the surface of an object under certain conditions. With the continuous expansion of the application range of the anticorrosive paint, the technical requirements are also continuously improved. When the anticorrosive paint is used, the coating film is easily damaged mechanically or chemically, and the following conditions are easy to occur: surface damage (e.g. scratches) of the coating film, cracks reaching the metal surface of the substrate, extensive flaking, discoloration, microcracks (also known as crazing in polymer physics). the self-repairing function of the coating is endowed, so that the problems in the use of the coating can be well solved.
In the self-repairing coating, based on the basic composition of the coating, the auxiliary agent type coating with a phase-splitting structure mainly comprises types such as capsules (capsules), fibrous fillers, layered intumescent fillers, nano kaolin and the like. The microcapsule self-repairing coating is prepared by encapsulating a repairing agent in microcapsules and compounding the microcapsules and a catalyst or a curing agent capable of polymerizing the repairing agent in a polymer material. When the interior of the polymer coating is damaged to generate micro-cracks, the microcapsules are broken under the action of the micro-cracks, wherein the coated repairing agent flows out under the action of siphonage and fills the interior of the micro-cracks, and the repairing agent reacts with a catalyst or a curing agent in the base material to initiate polymerization, so that the micro-cracks are repaired, and the performance of the coating is recovered to a certain degree. The microcapsule self-repairing coating is an important application field of an intelligent repairing material, and has very important significance for prolonging the service life of a body material.
At present, the microcapsule coating mainly comprises microcapsules with built-in repair agents in emulsion, wherein the emulsion is composed of epoxy resin and ethylenediamine, the repair agents are core material emulsion composed of the epoxy resin and sodium dodecyl benzene sulfonate, and the wall materials of the microcapsules are melamine-urea formaldehyde resin (MUF); the preparation method adopts an in-situ polymerization method, and the main process comprises the steps of firstly synthesizing melamine, urea, formaldehyde and triethanolamine into a MUF prepolymer, then adding a sodium dodecyl benzene sulfonate emulsifier into epoxy resin to prepare a core material emulsion, and then adjusting the mixed solution of the MUF prepolymer and the core material emulsion to a certain pH value through hydrochloric acid to obtain a product. The self-repairing coating has a self-repairing function on damages under different conditions, and a new requirement is undoubtedly put forward on the design of the coating, so that the development and development of a novel microcapsule self-repairing anticorrosive coating product are a challenge.
The Chinese invention patent application No. 201811480065.5 discloses a microcapsule self-repairing anticorrosive coating and a preparation method thereof, wherein the coating is composed of silicon dioxide microcapsules with built-in corrosion inhibitors in silicon-based emulsion; the method comprises the steps of mixing an ethyl orthosilicate cyclohexane solution and a corrosion inhibitor, adjusting the pH value of the mixture by using acid, stirring for reaction, filtering reaction liquid, adding a sodium dodecyl benzene sulfonate aqueous solution into the obtained organic-inorganic hybrid emulsion, stirring, sequentially carrying out solid-liquid separation, washing and drying on the obtained water-in-oil type core material emulsion to obtain a silicon dioxide microcapsule coated with the corrosion inhibitor, adding a metal platinum catalyst into silicon oil, stirring to obtain a silicon-based emulsion, mixing the silicon dioxide microcapsule coated with the corrosion inhibitor and the silicon-based emulsion, adding maleic anhydride monodecane into the mixture, and stirring for reaction to obtain the target product. The Chinese patent application No. 201910649137.2 discloses a preparation technology of a self-repairing and anti-corrosion coating, belonging to the technical field of high polymer materials and anti-corrosion coatings. The preparation method comprises the following steps: (1) mixing the water phase containing the emulsifier with the oil phase containing the vinyl polymer monomer, the repairing agent, the initiator and the organic solvent to form oil-in-water O/W type emulsion, and performing irradiation crosslinking or thermal crosslinking to form a microcapsule shell; (2) dropwise adding aniline into the dispersion liquid of the microcapsule shell obtained in the step (1), adding an aqueous solution containing an aniline initiator, and reacting to obtain a polyaniline microcapsule; (3) and mixing the polyaniline microcapsule with matrix resin to obtain the self-repairing and anti-corrosion coating.
In order to solve the problems that microcapsules in the self-repairing coating are poor in stability and short in service life, and the mobility and chemical activity of an oil core material emulsion are poor, so that the repairing rate is too low, a novel microcapsule self-repairing anticorrosive coating needs to be provided, and the repairing efficiency of the self-repairing anticorrosive coating is improved.
Disclosure of Invention
Aiming at the problems of low repair rate and complex production process of the existing microcapsule self-repairing anticorrosive coating, the invention provides the silicon dioxide microcapsule self-repairing anticorrosive coating and the preparation method thereof, so that the repair efficiency of the self-repairing anticorrosive coating is improved, the service life is prolonged, and the raw materials are low in price, simple in process and low in preparation cost.
In order to solve the problems, the invention adopts the following technical scheme:
the self-repairing anticorrosive coating is characterized in that an oil phase formed by a corrosion inhibitor and ether is dispersed in a water phase formed by ammonia water, an emulsifier and water, tetraethoxyethyl ortho-silicic acid is dropwise added to react to obtain an emulsion, then the emulsion is aged, washed and dried to obtain a self-repairing microcapsule material, and the microcapsule material, polyurethane emulsion, acrylic emulsion, a filler, a defoaming agent and a thixotropic agent are further uniformly stirred to prepare the self-repairing anticorrosive coating.
The corrosion inhibitor is one or the combination of more than two of 2-mercaptobenzothiazole, benzotriazole and derivatives thereof, tetrazole derivatives, thiadiazole derivatives and imidazole derivatives.
The emulsifier is at least one of Sodium Dodecyl Sulfate (SDS), Dodecyl Trimethyl Ammonium Bromide (DTAB), polyoxyethylene sorbitan (Tween20) and hexadecyl ammonium bromide.
The mass concentration of the polyurethane emulsion is 12%.
The mass concentration of the acrylic emulsion is 15%.
The filler is one or the combination of more than two of talc, barite and mica.
The defoaming agent is a polyether modified organic silicon defoaming agent;
the thixotropic agent is fumed silica.
The preparation method of the silicon dioxide microcapsule self-repairing anticorrosive coating is characterized by comprising the following specific steps of:
(1) adding the corrosion inhibitor into the ether, and uniformly dispersing to form an oil phase;
(2) dissolving ammonia water and an emulsifier in water to form a water phase, then adding the oil phase in the stirring process and uniformly dispersing, then dropwise adding tetraethoxy ethyl ortho-silicic acid and stirring for reaction to obtain an emulsion;
(3) aging the emulsion in a closed container, and then centrifugally washing and drying the obtained precipitated capsules to obtain a silica-coated corrosion inhibitor capsule material;
(4) uniformly stirring the silica-coated corrosion inhibitor capsule material, polyurethane emulsion, acrylic emulsion, filler, defoaming agent and thixotropic agent to obtain the silica capsule self-repairing anticorrosive coating.
In the step (1), in the preparation of the oil phase, the mass ratio of the ether to the corrosion inhibitor is 15-30: 1-2.
In the preparation of the emulsion in the step (2), the mass ratio of ammonia water, emulsifier, water, oil phase and tetraethoxy ethyl ortho-silicic acid is 1-3: 1-2: 30-50: 25-45: 2-5.
The reaction in the step (2) is carried out at room temperature for 0.5-1 h.
The aging temperature in the step (3) is 25-35 ℃, and the precipitation is 24-28 h.
In the preparation of the self-repairing anticorrosive coating in the step (4), the mass ratio of the silica-coated corrosion inhibitor capsule material, the polyurethane emulsion, the acrylic emulsion, the filler, the defoaming agent and the thixotropic agent is 5-10: 40-50: 25-40: 3-7: 0.2-0.5: 0.3-0.5.
The rotating speed of the high-speed stirring in the step (4) is 1500-1600r/min, and the stirring is 15-18 min.
According to the invention, the oil phase and the water phase are emulsified by using the emulsifier active agent to form an oil-in-water system, and the fluidity and the activity of the oily corrosion inhibitor can be improved after the oily corrosion inhibitor is coated, so that the self-repairing efficiency of the prepared self-repairing microcapsule in the coating is obviously improved. Tetraethoxy ethyl ortho-silicic acid is used as a silicon source, the silicon dioxide coated corrosion inhibitor is obtained through reaction to form a microcapsule material, after the silicon dioxide is coated, the loading capacity of the corrosion inhibitor can be improved, the self-repairing capability of the microcapsule is improved, the self-repairing efficiency is improved, the stability of the microcapsule can be effectively improved due to the good weather resistance and chemical stability of the silicon dioxide, and the service life is prolonged. The whole process is simple and easy to operate, the raw materials are low in price, and the preparation cost is low.
The existing microcapsule self-repairing anticorrosive coating has the problems of low repairing rate and complex production process, and the application of the coating is limited. In view of the above, the invention provides a silicon dioxide microcapsule self-repairing anticorrosive coating and a preparation method thereof, wherein a corrosion inhibitor is dissolved in ether to form an oil phase; dissolving ammonia water and an emulsifier in water to form a water phase, adding an oil phase into the water phase in the stirring process, continuously adding dropwise tetraethoxy ethyl ortho-silicic acid after dispersion, and reacting at room temperature to obtain an emulsion; aging the emulsion in a closed container, and centrifugally washing and drying the precipitated capsules to obtain a silicon dioxide coated corrosion inhibitor capsule material; and adding the silica-coated corrosion inhibitor capsule material into the polyurethane emulsion system coating to obtain the silica capsule self-repairing anticorrosive coating. The microcapsule material formed by the silicon dioxide coated corrosion inhibitor is added into the self-repairing anticorrosive coating provided by the invention, and the corrosion inhibitor has good fluidity, high activity and good stability, so that the self-repairing efficiency of the coating is improved, the service life is effectively prolonged, and the used material has the advantages of low price, simple process, low preparation cost and wide application prospect.
Compared with the prior art, the self-repairing anticorrosive coating of the silicon dioxide microcapsule and the preparation method thereof have the outstanding characteristics and excellent effects that:
1. according to the invention, the oily corrosion inhibitor is coated, so that the fluidity of the corrosion inhibitor can be improved, and the activity is high, thereby improving the self-repairing efficiency of the coating.
2. The invention further uses the microcapsule formed by silicon dioxide to directly coat the corrosion inhibitor, so that the process is simpler, and meanwhile, the corrosion inhibitor has high loading amount and good stability, so that the corrosion inhibitor has extremely long service life.
3. The raw materials used in the invention are all green environment-friendly materials, the price is low, the preparation process is simple, the preparation cost is greatly reduced, and the obtained product is extremely easy to be widely and commercially applied to the anticorrosion fields of steel structure buildings, concrete steel structures and the like.
Drawings
FIG. 1: a preparation process schematic diagram of the silica-coated corrosion inhibitor capsule material.
FIG. 2: FIG. 2 (a) shows a picture obtained when the repair is started in example 1, (b) shows a picture obtained after 24 hours of repair, and (c) shows a picture obtained after 72 hours of repair;
FIG. 3: fig. 3 (d) shows a picture immediately after repair in comparative example 1, (e) shows a picture after 24h of repair, and (f) shows a picture after 72h of repair.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding 1.5kg of 2-mercaptobenzothiazole into 22 kg of diethyl ether, and uniformly dispersing to form an oil phase;
(2) dissolving 2kg of ammonia water and 1.5kg of dodecyl trimethyl ammonium bromide in 40 kg of water to form a water phase, then adding 35kg of oil phase in the stirring process, uniformly dispersing, then dropwise adding 3.5 kg of tetraethoxy ethyl ortho-silicic acid, and reacting for 1 hour at room temperature to obtain emulsion;
(3) aging the emulsion in a closed container at the temperature of 30 ℃ for 26h, then centrifugally washing and drying the obtained precipitated capsules to obtain the silica-coated corrosion inhibitor capsule material;
(4) 2kg of silicon dioxide coated corrosion inhibitor capsule material, 15kg of polyurethane emulsion with the mass concentration of 12%, 10kg of acrylic emulsion with the mass concentration of 15%, 1.2kg of mica powder, 0.1kg of polyether modified organic silicon defoamer and 0.125kg of fumed silica are dispersed at a high speed of 1550r/min for 16min to obtain the silicon dioxide capsule self-repairing anticorrosive coating.
Example 2
(1) Adding 1.2kg of benzotriazole and derivatives thereof into 28 kg of diethyl ether, and uniformly dispersing to form an oil phase;
(2) dissolving 1.5kg of ammonia water and 1.2kg of sodium dodecyl sulfate in 45 kg of water to form a water phase, then adding 40 kg of oil phase in the stirring process, uniformly dispersing, then dropwise adding 2.5 kg of tetraethoxy ethyl ortho-silicic acid, and reacting at room temperature for 0.5h to obtain emulsion;
(3) aging the emulsion in a closed container at the temperature of 28 ℃ for 27h, then centrifugally washing and drying the obtained precipitated capsules to obtain a silica-coated corrosion inhibitor capsule material;
(4) 3kg of silicon dioxide coated corrosion inhibitor capsule material, 12kg of polyurethane emulsion with the mass concentration of 12%, 10kg of acrylic emulsion with the mass concentration of 15%, 1kg of talcum powder, 0.1kg of polyether modified organic silicon defoamer and 0.12kg of fumed silica are dispersed at a high speed of 1600r/min for 15min to obtain the silicon dioxide capsule self-repairing anticorrosive coating.
Example 3
(1) Adding 1.8kg of tetrazole derivative into 20 kg of ethyl ether, and uniformly dispersing to form an oil phase;
(2) dissolving 2.5 kg of ammonia water and 1.8kg of polyoxyethylene sorbitan ester in 35kg of water to form a water phase, then adding 30kg of oil phase in the stirring process, uniformly dispersing, dropwise adding 4 kg of tetraethoxyethyl ortho-silicic acid, and reacting at room temperature for 1 hour to obtain emulsion;
(3) aging the emulsion in a closed container at the temperature of 32 ℃ for 25h, then centrifugally washing and drying the obtained precipitated capsules to obtain a silica-coated corrosion inhibitor capsule material;
(4) 2kg of silicon dioxide coated corrosion inhibitor capsule material, 15kg of polyurethane emulsion with the mass concentration of 12%, 10kg of acrylic emulsion with the mass concentration of 15%, 1.5kg of mica powder, 0.1kg of polyether modified organic silicon defoamer and 0.1kg of fumed silica are dispersed at a high speed of 1500r/min for 18min to obtain the silicon dioxide capsule self-repairing anticorrosive coating.
Comparative example 1
Comparative example 1 in comparison with example 1, no corrosion inhibitor coated by silica was added, the others being identical with example 1.
The test method comprises the following steps:
self-repairing Performance test referring to GB/T1771-91 determination of neutral salt spray resistance of colored paint and varnish coating prepared in example 1 and comparative example 1, the coating is coated on a polished steel plate with the size of 100mm × mm, the polished steel plate is dried for 20 hours under the conditions of the temperature of 23 ℃ and the relative humidity of 50 percent, the polished steel plate is placed in an aging resistant test box for aging for 48 hours, then a 20mm × mm cross scratch is scratched at the center of the test plate by a single-blade cutter, the scratch is scratched through the coating to the bottom layer, and the polished steel plate is placed in a spray chamber of a salt spray test box, wherein the volume of the spray chamber is 1m3The test plate is arranged below a nozzle in the spray chamber, the surface to be tested faces upwards, the included angle between the test plate and the vertical line is 20 ℃, a top cover of the spray chamber is closed, a valve of a test solution storage tank is opened, the solution flows into the storage tank, the spraying is continuously carried out within 24 hours of the whole test period, and the damage phenomenon of the surface of the test plate is checked after the end of each test period.
The test results are detailed in fig. 2 and 3. FIG. 2 (a) shows a picture obtained when the repair is started in example 1, (b) shows a picture obtained after 24 hours of repair, and (c) shows a picture obtained after 72 hours of repair; fig. 3 (d) shows a picture immediately after repair in comparative example 1, (e) shows a picture after 24h of repair, and (f) shows a picture after 72h of repair.
As can be seen from FIGS. 2 to 3, after 24 hours, rust stains appear in both example 1 and comparative example 1, and the rust stains appearing in comparative example 1 are more than those in example 1, and the rust stains of example 1 are not enlarged any more after 72 hours, but the rust stains of comparative example 1 are obviously increased, which shows that the corrosion inhibitor can be slowly repaired by coating the silica microcapsule with the corrosion inhibitor, so that the corrosion inhibitor has extremely long service life.
Claims (9)
1. The self-repairing anticorrosive coating is characterized in that an oil phase formed by a corrosion inhibitor and ether is dispersed in a water phase formed by ammonia water, an emulsifier and water, tetraethoxyethyl ortho-silicic acid is dropwise added to react to obtain an emulsion, then the emulsion is aged, washed and dried to obtain a self-repairing microcapsule material, and the microcapsule material, polyurethane emulsion, acrylic emulsion, a filler, a defoaming agent and a thixotropic agent are further uniformly stirred to prepare the self-repairing anticorrosive coating.
2. The self-repairing anticorrosive coating of silica microcapsule according to claim 1,
the corrosion inhibitor is one or the combination of more than two of 2-mercaptobenzothiazole, benzotriazole and derivatives thereof, tetrazole derivatives, thiadiazole derivatives and imidazole derivatives;
the emulsifier is at least one of Sodium Dodecyl Sulfate (SDS), Dodecyl Trimethyl Ammonium Bromide (DTAB), polyoxyethylene sorbitan (Tween20) and hexadecyl ammonium bromide;
the mass concentration of the polyurethane emulsion is 12 percent;
the mass concentration of the acrylic emulsion is 15 percent;
the filler is one or the combination of more than two of talc, barite and mica;
the defoaming agent is a polyether modified organic silicon defoaming agent;
the thixotropic agent is fumed silica.
3. The preparation method of the silica microcapsule self-repairing anticorrosive coating as claimed in any one of claims 1 to 2, which is characterized by comprising the following steps:
(1) adding the corrosion inhibitor into the ether, and uniformly dispersing to form an oil phase;
(2) dissolving ammonia water and an emulsifier in water to form a water phase, then adding the oil phase in the stirring process and uniformly dispersing, then dropwise adding tetraethoxy ethyl ortho-silicic acid and stirring for reaction to obtain an emulsion;
(3) aging the emulsion in a closed container, and then centrifugally washing and drying the obtained precipitated capsules to obtain a silica-coated corrosion inhibitor capsule material;
(4) uniformly stirring the silica-coated corrosion inhibitor capsule material, polyurethane emulsion, acrylic emulsion, filler, defoaming agent and thixotropic agent to obtain the silica capsule self-repairing anticorrosive coating.
4. The preparation method of the silica microcapsule self-repairing anticorrosive coating as claimed in claim 3, wherein in the step (1) of preparing the oil phase, the mass ratio of ethyl ether to corrosion inhibitor is 15-30: 1-2.
5. The preparation method of the silicon dioxide microcapsule self-repairing anticorrosive coating as claimed in claim 3, wherein in the emulsion preparation in step (2), the mass ratio of ammonia water, emulsifier, water, oil phase and tetraethoxyethyl orthosilicate is 1-3: 1-2: 30-50: 25-45: 2-5.
6. The preparation method of the silica microcapsule self-repairing anticorrosive coating as claimed in claim 3, wherein the reaction in the step (2) is carried out at room temperature for 0.5-1 h.
7. The preparation method of the silica microcapsule self-repairing anticorrosive paint as claimed in claim 3, wherein the aging temperature in the step (3) is 25-35 ℃, and the precipitation time is 24-28 h.
8. The preparation method of the silica microcapsule self-repairing anticorrosive coating according to claim 3, wherein in the preparation of the self-repairing anticorrosive coating in the step (4), the mass ratio of the silica-coated corrosion inhibitor capsule material, the polyurethane emulsion, the acrylic emulsion, the filler, the defoaming agent and the thixotropic agent is 5-10: 40-50: 25-40: 3-7: 0.2-0.5: 0.3-0.5.
9. The preparation method of the silica microcapsule self-repairing anticorrosive coating as claimed in claim 3, wherein the rotation speed of the high-speed stirring in the step (4) is 1500-.
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