CN112391122A - Titanium-based polymer alloy high-temperature-resistant anticorrosive paint and preparation method thereof - Google Patents

Titanium-based polymer alloy high-temperature-resistant anticorrosive paint and preparation method thereof Download PDF

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CN112391122A
CN112391122A CN202110070005.1A CN202110070005A CN112391122A CN 112391122 A CN112391122 A CN 112391122A CN 202110070005 A CN202110070005 A CN 202110070005A CN 112391122 A CN112391122 A CN 112391122A
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titanium
resin
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易俊松
彭晓淳
张驰
周剑
齐福刚
匡知群
罗帅
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Hunan Bondzer Technology Co ltd
Zeiridium Foshan Industrial Technology Co ltd
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Zeiridium Foshan Industrial Technology Co ltd
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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
    • C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • C09D187/005—Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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    • C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block 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
    • C09D5/002—Priming paints
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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
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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
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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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
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L2205/00—Polymer mixtures characterised by other features
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Abstract

The invention provides a titanium-based polymer alloy high-temperature-resistant anticorrosive paint and a preparation method thereof. The invention takes hydroxyl organic titanium polymer as a base material, and prepares titanium-based polymer alloy copolymer (TPI, TPAI, TBMI) by modification and synthesis, which is used for manufacturing titanium-based polymer alloy high-temperature-resistant anticorrosive paint, and the paint has excellent high-temperature-resistant and corrosion-resistant properties and is mainly used for the inner coating protection of equipment of an industrial flue gas desulfurization system.

Description

Titanium-based polymer alloy high-temperature-resistant anticorrosive paint and preparation method thereof
Technical Field
The invention belongs to the technical field of new materials and production and application thereof, and particularly relates to a titanium-based polymer alloy high-temperature-resistant anticorrosive paint and a preparation method thereof.
Background
As is known, titanium is a very active metal element, has low density, high specific strength, good ductility, low thermal conductivity, high and low temperature resistance, no toxicity, no magnetism, wear resistance and corrosion resistance, is widely applied to various fields such as military industry, maritime industry, aviation, aerospace, civil use and the like, and is known as a structural material of outer space and ocean. Titanium is arranged in the element system of the subgroup IV (titanium group) in the periodic table of the chemical elements, and has an atomic number of 22, an atomic weight of 47.88 and a valence of +2, +3 and + 4. Thus, its reactivity also provides it with a reactive tendency to be diverse under certain environmental conditions.
The standard electrode potential of titanium is very low (E = -1.63V), and the passivation potential is also low, so that passivation is easy. At normal temperature, the surface of titanium is easy to form a passive film composed of oxide and nitride, which is very stable in atmosphere and many aggressive mediums and has good corrosion resistance. In the atmosphere, aqueous chloride solutions and oxidizing acids (nitric acid, chromic acid, etc.) and most organic acids, their corrosion resistance exceeds that of stainless steel; it is basically not corroded in seawater, so it is the most ideal material for ocean engineering.
However, titanium metal materials are expensive, and the popularization and application of titanium metal materials in the general industry, particularly the civil industry field, are always influenced.
If the metal titanium and the organic polymer material are grafted to form the polymer alloy state polymer and then the polymer alloy state polymer is popularized and applied to the field of industrial corrosion prevention in the form of a coating, the method is equivalent to plating a layer of corrosion-resistant titanium film on the surface of the metal, can replace stainless steel, solves the problem of industrial corrosion, can greatly reduce the manufacturing cost, and improves the economic benefit of enterprises, thus being the purpose and reason of the invention.
Titanium-based high molecular polymers (also known as polytitaxanes), which are generic names for metal polymers containing Titanium atoms in the main chain molecular structure, can be prepared from Titanium ortho-titanate Ti (OR)4After partial hydrolysis, the product is condensed. The titanium polysiloxane can be used as a surfactant, a water repellent agent and an antirust agent, and can form fibers under mechanical stirring; some of these are useful as heat resistant coatings, a precedent to the early use of organic titanium for coatings.
The invention relates to a technical method for preparing a nano organic titanium polymer by an invention patent (ZL200810029936.1) originally applied by the inventor, which is to prepare titanium hydride powder (TiH)2) Epoxy resin, catalyst (A)α-Al2O x3-) The nano dispersant, titanate coupling agent, silane coupling agent and mixed solvent are filled into a ball milling reaction tank for solid-liquid ball milling reaction, and the synthesized organic Titanium polymer (TPP-I) with epoxy groups is synthesized, wherein the reaction formula of the synthesized product is shown in figure 1. The polymer can only be used for preparing a crosslinking special coating by using an epoxy curing agent, so that certain limitation exists in application.
In the prior art, the traditional high-temperature-resistant anticorrosive paint mainly takes phenolic resin, furan resin, novolac epoxy resin, vinyl ester resin and organic silicon resin as film-forming matrixes, and the film-forming resins have insuperable defects, such as corrosion resistance of phenolic resin, furan, epoxy resin and vinyl resin, but the high-temperature resistance (less than or equal to 120 ℃) is limited; the organic silicon resin is high temperature resistant, the heat resistance limit value of the pure organic silicon resin can reach 300 ℃, but the organic silicon resin is not resistant to acid corrosion, especially acid corrosion in a high-temperature environment. Therefore, the coating product currently used cannot adapt to the acidic corrosion in the high-temperature environment, the coating can fail for several months under the extreme working condition, so that some desulfurization high-temperature equipment is corroded and leaks, and enterprises become rescue teams and stop leakage everywhere everyday. Thus, the prior art has certain limitations.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a titanium-based polymer alloy high-temperature-resistant anticorrosive coating and a preparation method thereof. The invention also provides application of the titanium-based polymer alloy copolymer in a high-temperature-resistant anticorrosive coating, and the coating has excellent high-temperature resistance and corrosion resistance and is mainly used for internal coating protection of equipment of an industrial flue gas desulfurization system.
A titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises raw materials of a titanium-based polymer alloy copolymer;
the titanium-based polymer alloy copolymer comprises the following raw materials in parts by weight:
400-500 parts of imide resin, 50-200 parts of N-methyl pyrrolidone, 100-300 parts of dimethylacetamide and 100-300 parts of hydroxyl organic titanium polymer;
the imide resin is one or more of soluble polyimide resin, polyamide-imide resin and bismaleimide resin;
the molecular formula of the hydroxyl organic titanium polymer is
Figure 329464DEST_PATH_IMAGE001
。
The titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based paint and comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight:
10-25 parts of titanium-based high-molecular alloy copolymer, 5-15 parts of phenyl silicone resin emulsion, 10-20 parts of poly (phenol-oxygen resin) emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 5-10 parts of cosolvent, 5-15 parts of aqueous graphene dispersion slurry with solid content of 5-10%, 5-45 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is soluble polyimide resin or polyamide-imide resin, and the titanium-based polymer alloy copolymer is a titanium-based polyimide polymer alloy copolymer or a titanium-based polyamide-imide polymer alloy copolymer;
the cosolvent is a mixed solvent of two or three of tetrahydrofuran, dimethylformamide, dimethylacetamide and N-methylpyrrolidone in any proportion;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating auxiliary agent comprises one or more than two of a dispersing agent, fumed silica, hydrated aluminum-magnesium silicate, organic bentonite, a defoaming agent, a leveling agent, an anti-flash rust agent, a corrosion inhibitor and a pH regulator;
the component B is a closed isocyanate curing agent; the mass ratio of the component A to the component B is 4-5: 1.
the titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises a component A and a component B, wherein when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based primer, the component A comprises the following raw materials in parts by mass:
10-15 parts of titanium-based high-molecular alloy copolymer, 5-10 parts of phenyl silicone resin emulsion, 10-15 parts of poly (phenol-oxygen resin) emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran, 2-5 parts of N-methyl pyrrolidone, 10-15 parts of aqueous graphene dispersion slurry with solid content of 5-10%, 0.5-2 parts of flash rust prevention agent, 1-3 parts of corrosion inhibitor, 0.1-0.5 part of pH regulator, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1.5 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 15-20 parts of anti-rust pigment and 5-10 parts of filler; the mass ratio of the component A to the component B is 5: 1;
the antirust pigment is active zinc powder or a composite phosphate antirust pigment;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the component A comprises the following raw materials in parts by mass:
20-25 parts of titanium-based polymer alloy copolymer, 10-15 parts of phenyl silicone resin emulsion, 15-20 parts of poly (phenol-oxygen) resin emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 5-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran, 2-5 parts of N-methyl pyrrolidone, 5-10 parts of water-based graphene dispersion slurry with solid content of 5-10%, 3-5 parts of carbon black, 5-15 parts of mica powder, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1.5 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.1-1 part of phenolic resin, 5-10 parts of N-methyl pyrrolidone, 5-10,α-1-3 parts of phase nano aluminum oxide; the mass ratio of the component A to the component B is 4: 1.
The preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises the following steps of:
uniformly mixing titanium-based high-molecular alloy copolymer, fully methylated amino resin, styrene-butadiene rubber emulsion, water-soluble phenolic resin, water-based graphene dispersion slurry, a dispersing agent, an anti-flash rust agent, a corrosion inhibitor, fumed silica, hydrated aluminum magnesium silicate, tetrahydrofuran, N-methyl pyrrolidone, a defoaming agent, a leveling agent and a filling material, grinding, adding a pH regulator, adjusting the pH of the system to 7-9, adding polyphenoxy resin emulsion, phenyl silicone resin emulsion and an anti-rust pigment, and uniformly mixing and dispersing;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the preparation method comprises the following steps:
titanium-based polymer alloy copolymer, water-soluble phenolic resin, fully methylated amino resin, tetrahydrofuran, N-methyl pyrrolidone, aqueous graphene dispersion slurry, carbon black, mica powder, fumed silica, hydrated aluminum magnesium silicate, a defoaming agent, a leveling agent, a dispersing agent, a,α-Grinding the phase nano-alumina after uniformly mixing, adding phenyl silicone resin emulsion, butadiene styrene rubber emulsion and poly phenol-oxygen resin emulsion, and uniformly mixing and dispersing.
The titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based paint and comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight:
18-23 parts of titanium-based polymer alloy copolymer, 13-18 parts of water-soluble phenolic resin, 8-13 parts of aqueous dispersion phenyl silicone resin, 10-20 parts of poly (phenol-oxygen) resin emulsion, 5-10 parts of styrene-butadiene rubber emulsion, 15-20 parts of antirust pigment, 3-35 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is soluble polyimide resin or polyamide-imide resin, and the titanium-based polymer alloy copolymer is a titanium-based polyimide polymer alloy copolymer or a titanium-based polyamide-imide polymer alloy copolymer;
the component B is a water-based isocyanate curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is characterized in that the antirust pigment is active zinc powder or a composite phosphate antirust pigment;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating additive comprises the following raw materials:
0.1-1 part of dispersing agent, 0.5-2.5 parts of anti-flash rust agent, 1-5 parts of corrosion inhibitor, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of hydrated aluminum magnesium silicate.
The preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises the following steps:
uniformly mixing the titanium-based polymer alloy copolymer, the water-soluble phenolic resin, the aqueous dispersion phenyl silicone resin, the anti-rust pigment, the pigment filler and the coating auxiliary agent, grinding, adding the poly (phenol-oxygen resin) emulsion and the styrene butadiene rubber emulsion, and uniformly mixing and dispersing.
The titanium-based polymer alloy high-temperature-resistant anticorrosive paint is oily paint and comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight:
10-30 parts of titanium-based polymer alloy copolymer, 8-15 parts of active diluent, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-20 parts of toughening wear-resistant material, 5-15 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is bismaleimide resin, and the titanium-based polymer alloy copolymer is titanium-based bismaleimide polymer alloy copolymer;
the active diluent is dicyclooxazole or 3-aminopropyl trihydroxy silane, or a mixture of the dicyclooxazole and the 3-aminopropyl trihydroxy silane in any proportion;
the toughening wear-resistant material is one or more than two of elastic saturated polyester resin, liquid nitrile rubber and liquid fluorosilicone rubber;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating auxiliary agent comprises one or more than two of wetting dispersant, defoamer, flatting agent, thickener and anti-settling agent;
the component B is an isocyanate HDI trimer curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
the titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises a component A and a component B, wherein when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is an oily primer, the component A comprises the following components in parts by mass:
10-20 parts of titanium-based polymer alloy copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxy silane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of liquid nitrile rubber, 10-20 parts of antirust pigment, 10-15 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organic bentonite; the mass ratio of the component A to the component B is 5: 1; the antirust pigment is phosphate or composite phosphate antirust pigment;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is an oily finish, the component A comprises the following components in parts by mass:
20-30 parts of titanium-based high-molecular alloy copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxysilane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of benzyl silicone resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of liquid nitrile rubber, 3-5 parts of carbon black, 5-10 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organobentonite; the mass ratio of the component A to the component B is 4: 1.
The preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises the following steps:
and uniformly mixing the raw materials in the component A in proportion, grinding, filtering and packaging.
The titanium-based high-molecular alloy high-temperature-resistant anticorrosive paint is mainly used for protecting industrial flue gas desulfurization system equipment in an extreme working condition corrosion environment, compared with the prior art, the paint product disclosed by the invention has excellent high-temperature resistance and corrosion resistance, breaks through the technical bottleneck of the extreme working condition environment, is corrosion-resistant and high-temperature-resistant (less than or equal to 300 ℃), is inspected in the equipment after being used for 5 years under the extreme working condition, is intact as before and can still ensure the normal operation of the equipment after being used for 8 years to the maximum extent, and does not need maintenance, so that the titanium-based high-molecular alloy high-temperature-resistant anticorrosive paint is popular and favored by users.
Drawings
FIG. 1 shows the synthesis reaction formula of an organic titanium polymer TPP-I with epoxy group mentioned in the background art.
FIG. 2 shows the reaction formula for synthesizing the hydroxy organic titanium polymer TPP-II of the present invention.
FIG. 3 shows the synthesis reaction formula of the titanium-based polymer alloy copolymer TPI of the present invention.
FIG. 4 is an FT-IR analysis spectrum of a raw material mixture of TPP-II before ball-milling reaction in the example of the invention.
FIG. 5 is an FT-IR characteristic spectrum of a raw material mixture of TPP-II in an embodiment of the invention after ball milling for 30h in a common solid-liquid reaction.
FIG. 6 is a comparative FT-IR analysis spectra before and after common solid-liquid reaction ball milling of the mixed materials of the example of the invention.
FIG. 7 is an FT-IR characteristic spectrum of TPP-II after ball milling for 3h by ultrasonic solid-liquid reaction of the mixed materials in the embodiment of the invention.
FIG. 8 is a graph comparing the effects of different ball milling methods.
FIG. 9 is an electron micrograph of TPP-II according to example of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention adopts poly phenol-oxygen resin (also called phenoxy resin) as matrix, and prepares hydroxyl organic titanium polymer with hydroxyl functional group by mechanochemical direct synthesis.
The embodiment of the invention prepares the hydroxyl organic titanium polymer, thereby expanding the application range of the nano organic titanium polymer. The method not only thins the micron-sized titanium hydride to be in a nanometer scale through the coupling effect of mechanical force and auxiliary ultrasonic waves, but also induces a high molecular polymer to generate a chain-breaking graft polymerization reaction, so that a polyphenoxy resin (also called phenoxy resin) is combined with titanium atoms to generate a hydroxyl organic titanium polymer (TPP-II). The reaction process of the synthesized product is shown in figure 2, and the molecular structural formula of the hydroxyl organic titanium polymer is shown as follows:
Figure 654135DEST_PATH_IMAGE002
。
the embodiment of the invention adopts novel poly (phenoxy) resin as a polymeric matrix to be directly mixed with titanium hydride (TiH)2) The surface block polymerization is adopted, the preparation process is simpler, and the production cost and the expense are greatly saved.
The hydroxyl organic titanium polymer comprises the following raw materials in parts by weight:
titanium hydride powder (TiH)2) 20-25 parts of phenoxy resin, 15-20 parts of DMF (dimethyl formamide), 8-12 parts of DMAC (dimethylacetamide), 15-20 parts of NMP (N-methylpyrrolidone), 5-10 parts of nano dispersant, 1-3 parts of titanate coupling agent and 1-3 parts of silane coupling agent.
Preferably, the raw material composition of the hydroxyl organic titanium polymer also comprises:γ-phase nano alumina (A)γ-Al2O x3-) 1-5 parts.
By addingγPhase nano alumina(s) (ii)γ-Al2O x3-) The method can accelerate the reaction rate of the hydroxyl organic titanium polymer and shorten the reaction time. Since the alumina is refined to the nano-scale, there will be a missing bond (oxygen-coordinated bond or oxygen-deficient bond), and therefore, in the embodiment of the present invention, it will be describedγ-Nano alumina is remarked asγ-Al2O x3-. By adding into the raw materialsγ-The phase nano alumina plays the role of a catalyst.
The invention utilizes the chemical activity of metallic titanium, under the action of mechanochemistry, the titanium hydride powder can initiate the chemical bond of the polymer and the surface lattice bond of titanium metal particles to break in the nano-processing procedure, so as to generate ions or groups with extremely high surface activity, so that the polymer is degraded into small molecular oligomers, and the grafting polymerization reaction can be carried out under high temperature and high pressure, thereby realizing the molecular structure reforming and forming a high molecular polymer with a brand new structure.
The preparation method of the hydroxyl organic titanium polymer comprises the following steps:
mixing the raw materials, ball-milling for 4-8 h, and simultaneously performing ball milling at the frequency of 40-50 KHz and the power of 100-300W and the power of 1-2W/cm3The intensity was ultrasonically assisted for dispersion.
Further, a planetary ultrasonic-assisted solid-liquid reaction ball milling device is adopted in the ball milling process, the ball milling conditions are that revolution is 18-168 r/min and rotation is 70-670 r/min, and after the ball milling is finished, the tank is opened and the materials are taken when the temperature is reduced to 40-50 ℃, so that the hydroxyl organic titanium polymer is obtained.
Furthermore, in the ball milling process, four graded zirconium balls (phi 5, phi 10, phi 15 and phi 20mm) are respectively filled in each ball milling tank to two thirds of the tank volume, and the volume ratio of ball materials is about 5-6: 1.
The embodiment of the invention is based on the mechanochemical principle, titanium hydride powder and phenoxy resin are blended, and the nano titanium base material is prepared by an ultrasonic-assisted solid-liquid reaction ball milling technology. Under the action of mechanical force, the polymer generates critical stress to break chemical bonds due to uneven internal stress distribution or impact energy concentrated on individual chain segments of the high-molecular polymer. The invention prepares the nanometer organic titanium high molecular polymer, which utilizes the characteristic that the main chain of the structure of the polyphenolic oxygen resin contains hetero atoms (-O-), generates chain breakage through the action of mechanochemistry and bonds with titanium atoms to form a metal polymer with a brand new structure.
The working principle of the planetary ultrasonic-assisted solid-liquid reaction ball milling device as a synthesis preparation tool is as follows: when the ultrasonic wave is applied, the plug of the ultrasonic generator is inserted into the socket of the energy converter, and simultaneously, the switch on the ultrasonic generator is turned on, at the moment, the energy converter starts to work, and the ultrasonic wave can be input. Because the ultrasonic wave has very strong penetrability, can penetrate the stainless steel plate with the thickness of 2mm, and has physical and chemical effects on the materials in the ball milling tank.
The invention utilizes the chemical activity of metallic titanium, under the action of mechanochemistry, the titanium hydride powder can initiate the chemical bond of the polymer and the surface lattice bond of titanium metal particles to break in the nano-processing procedure, so as to generate ions or groups with extremely high surface activity, so that the polymer is degraded into small molecular oligomers, and the grafting polymerization reaction can be carried out under high temperature and high pressure, thereby realizing the molecular structure reforming and forming a high molecular polymer with a brand new structure.
The invention also aims to prepare the titanium-based polymer alloy copolymer by using the hydroxyl organic titanium polymer (TPP-II) as a base material.
TPP-II is a titanium-based polymer material for modification, which can be used as an intermediate material, can be used as a coating film-forming substrate independently, or can be blended and copolymerized with various high polymers (such as EP, PY, PET, PI, EP-PF and the like) to prepare other high polymer copolymers, so that the TPP-II is generally called as a titanium-based macromolecular alloy (TMA).
The titanium-based polymer alloy copolymer comprises the following raw materials in parts by weight:
400-500 parts of imide resin, 50-200 parts of N-methyl pyrrolidone (NMP), 100-300 parts of Dimethylacetamide (DMAC) and 100-300 parts of hydroxyl organic titanium polymer;
when the imide resin is a soluble imide resin, the titanium-based polymer alloy copolymer is a titanium-based imide polymer alloy copolymer. The imide resin is one or more of soluble polyimide resin (PI), polyamide-imide resin (PAI) and bismaleimide resin (bismaleimide resin MBI for short).
Specifically, when the imide resin is soluble polyimide resin (PI), the obtained titanium-based polymer alloy copolymer is titanium-based polyimide polymer alloy copolymer (TPI), which is a water/oil universal titanium-based polyimide polymer alloy copolymer, and the synthetic reaction process is shown in fig. 3.
When the imide resin is polyamide imide resin (PAI), the obtained titanium-based polymer alloy copolymer is titanium-based polyamide imide polymer alloy copolymer (TPAI), is water/oil general-purpose titanium-based polyamide imide polymer alloy copolymer, and the synthetic reaction process is the same as the TPI and is not repeated. Compared with polyamide, polyamide-imide has an imide structure behind the polyamide structure, the reactable functional groups of the polyamide-imide and the polyamide structure are-NH, and the functional groups are used for grafting polymerization with a hydroxyl organic titanium copolymer when a titanium-based high polymer copolymer is synthesized, so that the properties of TPI and TPAI are basically the same, and the TPI is taken as an example for further explanation in the coating scheme of the embodiment of the invention.
When the imide resin is bismaleimide (bismaleimide MBI for short), the obtained titanium-based polymer alloy copolymer is titanium-based bismaleimide polymer alloy copolymer (TBMI), which is a solvent-type titanium-based bismaleimide polymer alloy copolymer, and the synthetic reaction process of the copolymer is the same as that of the TPI and is not repeated.
The main differences between TPI, TPAI and TBMI are reflected in the application: TPI and TPAI can be dissolved in polar solvent (such as NMP, DMF, DMAC, THF, acetone, etc.) and can be dissolved in water; TBMI is not co-soluble with water and is therefore limited in the manufacture of environmentally friendly coatings.
The preparation method of the titanium-based polymer alloy copolymer comprises the following steps:
taking imide resin, NMP and DMAC, mixing, stirring, heating until the imide resin is completely dissolved, adding a hydroxyl organic titanium polymer, heating to 100-140 ℃, and reacting at constant temperature for 2-4 hours to obtain the titanium-based polymer alloy copolymer.
The modified synthesized TPI, TPAI and TBMI titanium-based polymer alloy copolymer with hydroxyl organic titanium polymer as base material may be used in producing various titanium-based polymer alloy paint products. The raw materials with models in the embodiment scheme can be purchased in the chemical industry market.
The graphene dispersion slurry mentioned in the embodiment is divided into aqueous and oily types:
1) the preparation method of the aqueous graphene dispersion slurry comprises the following steps:
the water-based graphene dispersion slurry is water-soluble, comprises, by mass, 5-10% of graphene (powder), 5-10% of a nano hyper-dispersant, 2-4% of a silane coupling agent, 15-25% of a water-soluble resin, and the balance of a solvent (the solvent can be one or a mixture of more than two of DMF, MIBK, NMP and purified water), and is prepared by ultrasonic-assisted high-speed dispersion.
According to the water-based graphene dispersion slurry with the solid content of 5%, the addition amount of graphene (powder) (provided by Qingdada Detong New Material science and technology Co., Ltd.) is 5%, the addition amount of CI-913 nano ultra-dispersant is 8%, the addition amount of KH-560 silane coupling agent is 3%, the addition amount of MEA303 fully methylated amino resin is 20%, and the balance is solvent (50% of N-methylpyrrolidone (NMP) and 50% of purified water).
2) The preparation method of the oily graphene dispersion slurry comprises the following steps:
according to the mass percentage, 5-10% of graphene (powder), 5-10% of nano hyper-dispersant, 1-5% of silane coupling agent, 20-30% of epoxy resin, 1-3% of organic bentonite and the balance of (50% of PMA, 30% of MIBK and 20% of DAA) mixed solvent are mixed and stirred uniformly, then the mixture is dispersed and ground by a nano bead mill, the particle size of the material is detected by a nano laser particle sizer in the grinding process, and when D90 is less than or equal to 100nm, the mixture is packaged for standby.
According to the scheme of the specific embodiment of the invention, the adopted oily graphene dispersion slurry with the solid content of 5% is prepared by the following steps of adding 5% of graphene (powder) (provided by Qingdao Delong New Material science and technology Co., Ltd.), 8% of CI-913 nano hyper-dispersant, 3% of KH-540 silane coupling agent, 25% of NPEL-128 epoxy resin, 2% of SD-1 organic bentonite and the balance of mixed solvent (50% of PMA, 30% of MIBK and 20% of DAA) in percentage by mass.
In the following embodiments, the particle size of the mica powder may be 800 to 1250 mesh, and the particle size of the active zinc powder may be 800 to 1000 mesh.
The present invention is further illustrated by the following specific examples.
The first embodiment is as follows: preparation of hydroxy organic titanium polymer TPP-II
Taking 23 parts by mass of titanium hydride powder (TiH)2The particle size phi of the Ti powder is 1-5 mu m, and the content is not less than 99.5 percent of Katsumadai titanium hydride powder in Zhongzhou province), 18 parts of YP-50 polyphenoxy resin (chemical engineering in Kunshan nations), 12 parts of DMF (dimethyl formamide), 10 parts of DMAC (dimethyl acetamide), 18 parts of NMP (N-methyl pyrrolidone), 8 parts of CI-913 nano hyper-dispersant (Katsumadai Kagaku), and 3 parts of VK-L10γPhase nano alumina(s) (ii)γ-Al2O3-xParticle size of 10 or lessµm, Xuancheng crystal-like new material), 2 parts of NDZ-201 titanate coupling agent Sanian biology and 2 parts of silane coupling agent KH-560, uniformly mixing, and then uniformly filling into four ball-milling reaction tanks, wherein the grinding material in each ball-milling tank is one half of the tank capacity, then respectively filling four graded zirconium balls (phi 5, phi 10, phi 15 and phi 20mm) into each ball-milling tank to two thirds of the tank capacity, wherein the volume ratio of the ball materials is about 6: 1, sealing the ball-milling tanks, and starting ultrasonic waves and a ball-milling device to operate. The technical parameters of the ultrasonic-assisted solid-liquid reaction ball-milling device are set as follows:
(1) a planetary ball mill: revolution is 100 r/min (rotating disc); rotating at 300r/min (charging bucket); (2) ultrasonic frequency: 40 KHz; (3) ultrasonic power: 200W; (4) ultrasonic intensity: 1.13W/cm3。
Used in the examples of the present invention is TiH2The powder has no other residual impurities, so no H is generated in the ball milling process2The ball milling tank escapes, so that the ball milling tank is not dangerous, can continuously run for 6 hours and stop, and has the temperature of about 150 ℃ and the pressure of about 0.6MPa in the ball milling tank. And (3) opening an exhaust valve to release pressure when the temperature in the tank is cooled to 40-50 ℃, and opening the tank to take the material, thereby obtaining the black viscous liquid-state hydroxyl organic titanium polymer (TPP-II).
Example two: synthesis of Ti-base high-molecular alloy copolymer TPI or TPAI
Weighing 500g of PY1005T soluble polyimide powder resin (Suzhou brand name photoelectricity technology), NMP100g and DMAc200g, adding the materials into a synthesis device with mechanical stirring, heating to 80 ℃ to completely dissolve the polyimide, adding 200g of TPP-II base material, heating to 120 ℃, controlling the constant temperature, and continuously reacting for 3 hours to obtain the titanium-based polyimide copolymer (TPI).
500g of PY9006T polyamidoimide resin (Suzhou brand name photoelectricity technology), 100g of NMP100g and 200g of DMAc200g are weighed and added into a synthesis device with mechanical stirring, then the temperature is raised to 80 ℃ to completely dissolve the polyamidoimide, 200g of TPP-II base material is added, the temperature is raised to 120 ℃, the constant temperature is controlled, and the reaction is continued for 3 hours, so that the titanium-based polyimide copolymer (TPAI) is obtained.
Example three: synthesis of titanium-based polymer alloy copolymer TBMI
Weighing 500g of BMI bismaleimide resin (bismaleimide resin for short, new Honghu bismaleimide material), 100g of NMP100g and 200g of DMF200g, adding into a synthesis device with mechanical stirring, heating to 80 ℃ to completely dissolve BMI, adding 200g of TPP-II base material, heating to 120 ℃, controlling the constant temperature, and continuously reacting for 3 hours to obtain the titanium-based bismaleimide copolymer (TBMI).
The technical index parameters of TPP-II, TPI, TPAI and TBMI obtained by the preparation are listed in Table 1.
TABLE 1 main technical indices of TPP-II, TPI, TBMI
Figure 319603DEST_PATH_IMAGE003
In order to verify the difference between mechanochemical effect and the above products, the present invention performed IR and TEM analysis on each of the above products prepared, and the test results are shown in fig. 4 to 9.
FIG. 4 is a FT-IR characteristic spectrum of a sample before ball-milling reaction of a raw material mixture of TPP-II in the embodiment of the invention, FIG. 5 is a FT-IR characteristic spectrum of a sample after ball-milling of a raw material mixture of TPP-II for 30h (without ultrasonic treatment) in a common solid-liquid reaction, FIG. 6 is a comparison graph of two groups of results of FIGS. 4 and 5, wherein the upper graph is the graph of FIG. 4, and the lower graph is the graph of FIG. 5, and it can be seen from FIG. 6 that the two graphs are not greatly different, no characteristic peak appears yet, which indicates that the blended material has not undergone chemical change, but has been refined.
FIG. 7 is an infrared spectrogram of TPP-II after ball milling for 3h through ultrasonic solid-liquid reaction of the mixed material in the embodiment of the invention, as can be seen from the chart, many original characteristic peaks are weakened or disappeared, new characteristic peaks appear, the change is obvious when comparing FIG. 4 with FIG. 7, which shows that the material has a chemical structure change, and FIG. 7 can be used as TPI-a characteristic ir spectrum of II. Comparing the characteristic infrared spectrum of TPI with the characteristic infrared spectrum of TBMI (not shown in the figure) at 500-1500 cm-1The segments have obvious similarities; at 2000cm-1To 4000cm-1Two to three distinct characteristic peaks appear in a section, particularly 2361cm-1The other two characteristic peaks are absorption peaks of interference of the catalyst and the coupling agent.
Fig. 8 is a comparison graph of effects of different ball milling modes, wherein a is a material particle size distribution graph of a raw material mixture of TPP-II in a common solid-liquid reaction ball mill for 6 hours, b is a material particle size distribution graph of a raw material mixture of TPP-II in a common solid-liquid ball mill for 30 hours, and c is a material particle size distribution graph of an ultrasonic-assisted solid-liquid ball mill for 3 hours in the embodiment. As can be seen from FIG. 8, by adopting the preparation method of the embodiment of the invention, the raw material can be rapidly nanocrystallized, and the particle size of the material can reach 10-100 nm within 3 hours under the condition of ultrasonic-assisted ball milling.
FIG. 9 is an electron microscope contrast view of TPP-II, wherein, a is an SEM image of a titanium base material TPP-II in a dispersed state after ultrasonic solid-liquid reaction ball milling, b is a TEM image of the titanium base material TPP-II in a dispersed state after ultrasonic solid-liquid reaction ball milling, c is a TEM image of a mixed material without ball milling, and d is a TEM image of the TPP-II after ultrasonic solid-liquid reaction ball milling. As can be seen from the comparison of the pictures, the titanium base material TPP-II is uniformly dispersed and uniformly coated by the auxiliary agent.
Example four: preparation of water-based titanium-based polymer alloy high-temperature-resistant anticorrosive paint
In the prior art, flue gas desulfurization is already necessary for various large thermal power plants in the aspect of environmental protection treatment, and wet desulfurization is generally adopted in the plants. The wet desulphurization has many advantages, such as good desulphurization and denitration effects, PM2.5 dust cleaned, low treatment cost and the like, but has the inevitable disadvantage that the stripped sulphur and nitrate generate dilute sulphuric acid, sulphurous acid and nitric acid after meeting water, and the equipment and facilities of the desulphurization system are seriously corroded. This is the acidic corrosion condition in high temperature environment.
The embodiment provides a titanium-based polymer alloy high-temperature-resistant anticorrosive coating, which is prepared by taking a titanium-based polymer alloy copolymer (titanium-based copolymer for short) TPI or TPAI as one of main raw materials and compounding with auxiliary resin, pigment and filler, coating additives and the like. The coating consists of A, B two components and can be divided into a primer and a finish.
Specifically, the titanium-based polymer alloy high-temperature-resistant anticorrosive coating provided in the embodiment is a water-based coating, and comprises a component A and a component B, wherein the component A is a paint vehicle, the component B is an enclosed isocyanate curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
the component A comprises the following raw materials in parts by weight:
10-25 parts of titanium-based polymer alloy copolymer TPI or TPAI, 5-15 parts of phenyl silicone resin emulsion, 10-20 parts of poly (phenol-oxygen) resin emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 5-10 parts of cosolvent, 5-15 parts of water-based graphene dispersion slurry with solid content of 5-10%, 5-45 parts of pigment and filler and 3-8 parts of coating additive.
The cosolvent is a mixed solvent of two or three of tetrahydrofuran, dimethylformamide, dimethylacetamide and N-methylpyrrolidone in any proportion.
The pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate.
The coating auxiliary agent comprises one or more than two of a dispersing agent, fumed silica, hydrated aluminum-magnesium silicate, organic bentonite, a defoaming agent, a leveling agent, an anti-flash rust agent, a corrosion inhibitor and a pH regulator.
When the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based primer, the component A comprises the following raw materials in parts by mass:
10-15 parts of titanium-based polymer alloy copolymer TPI or TPAI, 5-10 parts of phenyl silicone resin emulsion, 10-15 parts of polyphenoxy resin emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran (NMF), 2-5 parts of N-methyl pyrrolidone, 10-15 parts of aqueous graphene dispersion slurry with solid content of 5-10%, 0.5-2 parts of flash rust inhibitor, 1-3 parts of corrosion inhibitor, 0.1-0.5 part of pH regulator, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1.5 parts of dispersant, 0.1-1 part of defoamer, 0.1-1 part of flatting agent, 15-20 parts of antirust pigment and 5-10 parts of filler;
the mass ratio of the component A to the component B is 5: 1;
the antirust pigment is active zinc powder or a composite phosphate antirust pigment; the composite phosphate antirust pigment comprises one or more than two of aluminum tripolyphosphate or composite zinc phosphate. In the embodiment of the invention, the antirust pigment adopts active zinc powder, and the filler adopts mica powder.
When the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based primer, the preparation method comprises the following steps: uniformly mixing titanium-based high-molecular alloy copolymer TPI or TPAI, fully methylated amino resin, styrene-butadiene rubber emulsion, water-soluble phenolic resin, aqueous graphene dispersion slurry, a dispersing agent, an anti-flash rust agent, a corrosion inhibitor, fumed silica, hydrated aluminum magnesium silicate, tetrahydrofuran, N-methyl pyrrolidone, a defoaming agent, a leveling agent and a filling material, grinding, adding a pH regulator after grinding to reach the required fineness (less than or equal to 35 mu m), adjusting the pH of the system to 7-9, then adding polyphenoxy resin emulsion, phenyl silicone resin emulsion and an anti-rust pigment, and uniformly mixing and dispersing. Wherein, during grinding, a proper amount of purified water can be added to adjust the viscosity of the system so as to be suitable for the grinding state. The component B is uniformly mixed with the component A in proportion before the coating is used.
When the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the component A comprises the following raw materials in parts by mass:
20-25 parts of titanium-based polymer alloy copolymer TPI or TPAI, 10-15 parts of phenyl silicone resin emulsion, 15-20 parts of polyphenoxy resin emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 5-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran (NMF), 2-5 parts of N-methyl pyrrolidone, 5-10 parts of water-based graphene dispersion slurry with solid content of 5-10%, 3-5 parts of carbon black, 5-15 parts of mica powder, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1 part of dispersant5 parts, 0.1 to 1 part of defoaming agent, 0.1 to 1 part of flatting agent,α-Phase nano alumina (A)α-Al2O x3-) 1-3 parts;
the mass ratio of the component A to the component B is 4: 1.
When the water-based titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the preparation method comprises the following steps: titanium-based polymer alloy copolymer TPI or TPAI, water-soluble phenolic resin, fully methylated amino resin, NMF, N-methyl pyrrolidone, water-based graphene dispersion slurry, carbon black, mica powder, fumed silica, hydrated aluminum magnesium silicate, a defoaming agent, a leveling agent, a dispersing,α-Al2O x3-Grinding to required fineness (less than or equal to 25 μm), adding phenyl silicone resin emulsion, styrene-butadiene rubber emulsion and poly (phenol-oxygen resin) emulsion, mixing, dispersing, filtering, and packaging. Wherein, during grinding, a proper amount of purified water can be added to adjust the viscosity of the system so as to be suitable for the grinding state. The component B is uniformly mixed with the component A in proportion before the coating is used.
In the specific implementation process, the surface of the object can be coated with a primer firstly and then coated with a finish, so that the performance effect of a paint film is best.
The coating is further illustrated by the following specific examples.
Primer (a component): taking 13 parts of TPI titanium-based copolymer, 8 parts of 2130 water-soluble phenolic resin (Zhengzhou Hengtong chemical industry), 10 parts of aqueous Graphene Dispersion Slurry (GDS) with the solid content of 5%, 7 parts of AL-1002 styrene-butadiene rubber emulsion (Japan Acyulong), 6 parts of cyanote 303 fully methylated amino resin, 3 parts of NMF, 4 parts of N-methyl pyrrolidone, 1.0 part of F2M flash rust inhibitor (DeTAC company), 1.0 part of HD-420 corrosion inhibitor, 0.8 part of A200 fumed silica, 1.0 part of Tolsa S9 hydrated aluminum magnesium silicate, 0.5 part of BYK-190 dispersant, 0.5 part of BYK-028 defoamer, 0.5 part of BYK-381 leveling agent and 7 parts of 800-mesh mica powder by mass; the components are mixed evenly and ground by a sand mill, a proper amount of water can be added to adjust the viscosity of the system to be suitable for the grinding state, after the grinding reaches the required fineness, 0.3 part of AMP-95pH regulator is added, the system is adjusted to the pH8, 8 parts of SH-9608 phenyl silicone resin emulsion (New four seas chemical industry in Hubei), 12 parts of PKHW-38 polyphenoxy resin emulsion and 17 parts of 1000-mesh active zinc powder are added, and the components are mixed and dispersed evenly under the low shearing state and packaged for later use.
Finishing coat (component A): by mass, 22 parts of TPI titanium-based copolymer, 7 parts of 2130 water-soluble phenolic resin, 5 parts of cyanote 303 fully methylated amino resin, 3.5 parts of NMF, 3 parts of N-methyl pyrrolidone, 8 parts of water-based graphene dispersion slurry with the solid content of 5%, 4 parts of pigment carbon black, 13 parts of 1250-mesh mica powder, 0.8 part of A200 fumed silica, 1.2 parts of Tolsa S9 hydrated aluminum magnesium silicate, 0.6 part of BYK-190 dispersing agent, 0.8 part of BYK-028 defoaming agent, 0.8 part of BYK-381 flatting agent, and the like,α-Al2O x3-2 parts of (1); the components are mixed evenly and ground by a sand mill, a proper amount of water can be added to adjust the viscosity of the system to be suitable for the grinding state, 12 parts of SH-9608 phenyl silicone resin emulsion, 7 parts of AL-1002 styrene-butadiene rubber emulsion (Nippon Aiyulong) and 17 parts of PKHW-38 polyphenolic oxide resin emulsion are added after the grinding reaches the required fineness, and the components are mixed, dispersed evenly, filtered and packaged.
The component B is a curing agent of a primer and a finish paint, and a BL3175 closed curing agent is directly selected. The primer comprises the following components in percentage by mass: group A: group B = 5: 1; the mass ratio of the finish paint is as follows: group a: group B = 4: 1.
The performance test results of the high-temperature resistant anticorrosive paint of the aqueous titanium-based polymer alloy are shown in Table 2.
Example five: preparation of bottom-surface-integrated water-based titanium-based polymer alloy high-temperature-resistant anticorrosive paint
In this embodiment, another aqueous titanium-based polymer alloy high-temperature-resistant anticorrosive paint is provided, which uses a titanium-based polymer alloy copolymer (abbreviated as titanium-based copolymer) TPI or TPAI as one of the main raw materials, and the paint product of this embodiment is a primer-topcoat one-in-one type paint, which is a package of a component a and a component B.
Specifically, the high-temperature-resistant anticorrosive coating of the aqueous titanium-based polymer alloy provided in the embodiment comprises a component A and a component B, wherein the component A is a paint vehicle, the component B is an aqueous isocyanate curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
the component A comprises the following raw materials in parts by weight:
18-23 parts of titanium-based polymer alloy copolymer TPI or TPAI, 13-18 parts of water-soluble phenolic resin, 8-13 parts of aqueous dispersion phenyl silicone resin, 10-20 parts of poly (phenoxy) resin emulsion, 5-10 parts of styrene-butadiene rubber emulsion, 15-20 parts of anti-rust pigment, 3-35 parts of pigment and filler and 3-8 parts of coating additive.
The antirust pigment is active zinc powder or a composite phosphate antirust pigment; the composite phosphate antirust pigment comprises one or a mixture of aluminum tripolyphosphate and composite zinc phosphate.
The pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate.
The coating auxiliary agent comprises one or more than two of a dispersing agent, an anti-flash rust agent, a corrosion inhibitor, a defoaming agent, a leveling agent, fumed silica and hydrated aluminum magnesium silicate.
Further, the coating auxiliary agent comprises the following raw materials:
0.1-1 part of dispersing agent, 0.5-2.5 parts of anti-flash rust agent, 1-5 parts of corrosion inhibitor, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of hydrated aluminum magnesium silicate.
The preparation method of the water-based titanium-based polymer alloy high-temperature-resistant anticorrosive paint comprises the following steps: uniformly mixing titanium-based high-molecular alloy copolymer, water-soluble phenolic resin, aqueous dispersion phenyl silicone resin, anti-rust pigment, pigment filler and coating auxiliary agent, grinding, adding appropriate amount of water to adjust the viscosity of the system to be suitable for a grinding state, grinding to reach a required fineness (less than or equal to 25 mu m), adding polyoxyl resin emulsion and butadiene styrene rubber emulsion, uniformly mixing and dispersing, filtering and packaging. The component B is uniformly mixed with the component A in proportion before the coating is used.
The coating is further illustrated by the following specific examples.
Primer-topcoat coating (component A): by mass, taking 20 parts of TPI titanium-based copolymer, 15 parts of 2130 water-soluble phenolic resin, 10 parts of JY8742 aqueous dispersion phenyl silicone resin, 0.5 part of BYK-190 dispersant, 1 part of F2M anti-flash rust agent (DeTAC company), 3.5 parts of HD-420 corrosion inhibitor, 0.5 part of BYK-028 defoaming agent, 0.5 part of BYK-381 leveling agent, 16 parts of PZ20 (France/Guangzhou Huanhu chemical industry) composite zinc-calcium phosphate antirust pigment, 3 parts of AM-100 pigment carbon black, 5 parts of 1250-mesh mica powder, 1 part of A200 fumed silica and 1 part of Tolsa S9 hydrated aluminum magnesium silicate; the components are mixed evenly and ground by a sand mill, a proper amount of water can be added to adjust the viscosity of the system to be suitable for the grinding state, after the grinding reaches the required fineness, 15 parts of PKHW-38 polyphenolic oxygen resin emulsion and 8 parts of SN-307R styrene-butadiene rubber emulsion are added, and the mixture is cut, mixed and dispersed evenly under the low shear state, filtered and packaged for later use.
The component B is Bayer 3100 aqueous isocyanate curing agent and is packaged separately.
The primer-topcoat water-based high-temperature-resistant anticorrosive coating comprises the following components in parts by weight: group a: group B = 4: 1.
The performance test results of the high-temperature resistant anticorrosive paint of the aqueous titanium-based polymer alloy are shown in Table 2.
TABLE 2 detection results of high temperature resistant coating performance of aqueous titanium-based polymer alloy
Figure 870670DEST_PATH_IMAGE004
EXAMPLE VI preparation of high-solid Ti-based Polymer alloy coating for flue gas desulfurization System
The scheme of the embodiment provides a titanium-based polymer alloy high-temperature-resistant anticorrosive paint, which is an oily paint, is a high-solid oily titanium-based polymer alloy paint for a flue gas desulfurization system, and is a bi-component (A/B group) self-drying curing type high-temperature-resistant anticorrosive paint prepared by compounding a titanium-based polymer alloy copolymer (TBMI) serving as a main film forming material with auxiliary resin, pigment and filler, a paint auxiliary agent, an active diluent and the like.
Specifically, the high-solid titanium-based polymer alloy coating for the flue gas desulfurization system provided in the embodiment of the present invention has a component a, and the component a comprises the following raw materials in parts by mass:
10-30 parts of TBMI titanium-based copolymer, 8-15 parts of active diluent, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-20 parts of toughening wear-resistant material, 5-15 parts of pigment and filler and 3-8 parts of coating additive.
Wherein the active diluent is dicyclooxazole or 3-aminopropyl trihydroxy silane, or a mixture of the dicyclooxazole and the 3-aminopropyl trihydroxy silane in any proportion.
The toughening wear-resistant material is one or more than two of elastic saturated polyester resin, Liquid Nitrile Butadiene Rubber (LNBR) and liquid fluorosilicone rubber.
The pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate.
The coating auxiliary agent comprises one or more than two of wetting dispersant, defoamer, flatting agent, thickener and anti-settling agent; the thickening agent can be organic bentonite, and the anti-settling agent can be fumed silica.
Further, the coating auxiliary agent comprises the following raw materials:
0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organic bentonite.
The high-solid titanium-based polymer alloy coating of the flue gas desulfurization system can also comprise a component B, wherein the mass ratio of the component A to the component B is (4-5): 1. the component B is an isocyanate curing agent and can be an isocyanate HDI trimer curing agent.
The high-solid titanium-based polymer alloy coating of the flue gas desulfurization system can be used as a primer and a finish according to the use application.
When the high-solid titanium-based polymer alloy coating of the flue gas desulfurization system is used as a primer, the component A comprises the following components in parts by mass:
10-20 parts of TBMI titanium-based copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxy silane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of Liquid Nitrile Butadiene Rubber (LNBR), 10-20 parts of antirust pigment, 10-15 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organic bentonite; the mass ratio of the component A to the component B is 5: 1. Wherein the antirust pigment is phosphate or composite phosphate antirust pigment.
When the high-solid titanium-based polymer alloy coating of the flue gas desulfurization system is used as a finish, the component A comprises the following components in parts by mass:
20-30 parts of TBMI titanium-based copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxysilane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of benzyl silicone resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of Liquid Nitrile Butadiene Rubber (LNBR), 3-5 parts of carbon black, 5-10 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organobentonite; the mass ratio of the component A to the component B is 4: 1.
The preparation method of the high-solid titanium-based polymer alloy coating of the flue gas desulfurization system comprises the following steps: the raw materials in the component A are uniformly mixed according to a proportion, ground to required fineness (the primer is less than or equal to 40 mu m, and the finish paint is less than or equal to 25 mu m), filtered and packaged. The component B is uniformly mixed with the component A in proportion before the coating is used.
In the specific implementation process, the surface of the object can be coated with a primer firstly and then coated with a finish, so that the performance effect of a paint film is best.
The coating is further illustrated by the following specific examples.
1. Primer (a component): taking 15 parts of TBMI copolymer, 7 parts of 3-aminopropyl trihydroxysilane, 8 parts of ALT-202 bicyclo oxazolidine, 10 parts of YP-50 phenoxy resin, 8 parts of YDJ-26 LNBR glue solution, 10 parts of NPCN-704 epoxy phenolic resin, 8 parts of D670 elastic saturated polyester resin, 18 parts of PZ20 composite phosphate antirust pigment, 12 parts of 800-mesh mica powder, 1 part of FR-0516 wetting dispersant, 0.5 part of BYK-052 defoaming agent, 0.5 part of BYK-306 flatting agent, 1 part of Y200 fumed silica and 1 part of SD-1 organic bentonite in parts by mass; sequentially putting into a container, placing in a high-speed dispersion machine for dispersion, grinding to required fineness by a sand mill after uniform mixing, and filtering and packaging by using 200-mesh filter cloth.
2. Finishing coat (component A): taking 25 parts of TBMI titanium-based copolymer, 7 parts of 3-aminopropyl trihydroxysilane, 8 parts of ALT-202 bicyclo oxazolidine, 10 parts of YP-50 phenoxy resin, 10 parts of NPCN-704 epoxy phenolic resin, 10 parts of 9806 phenylmethyl silicone resin, 8 parts of D670 elastic saturated polyester resin, 5 parts of YDJ-26 liquid nitrile rubber, 3 parts of MA-100 pigment carbon black, 10 parts of 800-mesh mica powder, 1 part of FR-0516 wetting dispersant, 0.5 part of BYK-052 defoaming agent, 0.5 part of BYK-306 flatting agent, 1 part of Y200 fumed silica and 1 part of SD-1 organic bentonite by mass; sequentially putting into a container and placing in a high-speed dispersion machine for dispersion, grinding by a sand mill after uniform mixing, and then filtering and packaging by filter cloth of 200 meshes.
The curing agent for the bottom coat and the top coat (component B) are both TH-100 HDI trimer curing agents and can be directly subpackaged. The mass ratio of the primer to the curing agent is as follows: group A: group B = 5: 1; the mass ratio of the finish paint is as follows: group a: group B = 4: 1. The coating system can be cured at normal temperature (20-30 ℃).
The performance test results of the high-solid titanium-based polymer alloy coating for the flue gas desulfurization system are shown in table 3.
TABLE 3 Performance test results of high-solid Ti-based polymer alloy coating for flue gas desulfurization system
Figure 997895DEST_PATH_IMAGE005
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that the modifications and equivalents of the specific embodiments of the present invention can be made by those skilled in the art after reading the present specification, but these modifications and variations do not depart from the scope of the claims of the present application.

Claims (10)

1. The high-temperature-resistant anticorrosive paint of the titanium-based polymer alloy is characterized in that raw materials of the high-temperature-resistant anticorrosive paint of the titanium-based polymer alloy comprise a titanium-based polymer alloy copolymer;
the titanium-based polymer alloy copolymer comprises the following raw materials in parts by weight:
400-500 parts of imide resin, 50-200 parts of N-methyl pyrrolidone, 100-300 parts of dimethylacetamide and 100-300 parts of hydroxyl organic titanium polymer;
the imide resin is one or more of soluble polyimide resin, polyamide-imide resin and bismaleimide resin;
the molecular formula of the hydroxyl organic titanium polymer is
Figure 682307DEST_PATH_IMAGE001
。
2. The titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 1, wherein the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based paint comprising a component A and a component B;
the component A comprises the following raw materials in parts by weight:
10-25 parts of titanium-based high-molecular alloy copolymer, 5-15 parts of phenyl silicone resin emulsion, 10-20 parts of poly (phenol-oxygen resin) emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 5-10 parts of cosolvent, 5-15 parts of aqueous graphene dispersion slurry with solid content of 5-10%, 5-45 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is soluble polyimide resin or polyamide-imide resin, and the titanium-based polymer alloy copolymer is a titanium-based polyimide polymer alloy copolymer or a titanium-based polyamide-imide polymer alloy copolymer;
the cosolvent is a mixed solvent of two or three of tetrahydrofuran, dimethylformamide, dimethylacetamide and N-methylpyrrolidone in any proportion;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating auxiliary agent comprises one or more than two of a dispersing agent, fumed silica, hydrated aluminum-magnesium silicate, organic bentonite, a defoaming agent, a leveling agent, an anti-flash rust agent, a corrosion inhibitor and a pH regulator;
the component B is a closed isocyanate curing agent; the mass ratio of the component A to the component B is 4-5: 1.
3. the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 2, wherein when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based primer, the component A comprises the following raw materials in parts by mass:
10-15 parts of titanium-based high-molecular alloy copolymer, 5-10 parts of phenyl silicone resin emulsion, 10-15 parts of poly (phenol-oxygen resin) emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 3-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran, 2-5 parts of N-methyl pyrrolidone, 10-15 parts of aqueous graphene dispersion slurry with solid content of 5-10%, 0.5-2 parts of flash rust prevention agent, 1-3 parts of corrosion inhibitor, 0.1-0.5 part of pH regulator, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1.5 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 15-20 parts of anti-rust pigment and 5-10 parts of filler; the mass ratio of the component A to the component B is 5: 1;
the antirust pigment is active zinc powder or a composite phosphate antirust pigment;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the component A comprises the following raw materials in parts by mass:
20-25 parts of titanium-based polymer alloy copolymer, 10-15 parts of phenyl silicone resin emulsion, 15-20 parts of poly (phenol-oxygen) resin emulsion, 5-10 parts of water-soluble phenolic resin, 5-10 parts of styrene-butadiene rubber emulsion, 5-8 parts of fully methylated amino resin, 2-5 parts of tetrahydrofuran, 2-5 parts of N-methyl pyrrolidone, 5-10 parts of water-based graphene dispersion slurry with solid content of 5-10%, 3-5 parts of carbon black, 5-15 parts of mica powder, 0.5-2 parts of fumed silica, 1-3 parts of hydrated aluminum magnesium silicate, 0.5-1.5 parts of dispersing agent, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.1-1 part of phenolic resin, 5-10 parts of N-methyl pyrrolidone, 5-10,α-1-3 parts of phase nano aluminum oxide; the mass ratio of the component A to the component B is 4: 1.
4. The titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 1, wherein the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based paint comprising a component A and a component B;
the component A comprises the following raw materials in parts by weight:
18-23 parts of titanium-based polymer alloy copolymer, 13-18 parts of water-soluble phenolic resin, 8-13 parts of aqueous dispersion phenyl silicone resin, 10-20 parts of poly (phenol-oxygen) resin emulsion, 5-10 parts of styrene-butadiene rubber emulsion, 15-20 parts of antirust pigment, 3-35 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is soluble polyimide resin or polyamide-imide resin, and the titanium-based polymer alloy copolymer is a titanium-based polyimide polymer alloy copolymer or a titanium-based polyamide-imide polymer alloy copolymer;
the component B is a water-based isocyanate curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
5. the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 4, wherein the antirust pigment is active zinc powder or a composite phosphate antirust pigment;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating additive comprises the following raw materials:
0.1-1 part of dispersing agent, 0.5-2.5 parts of anti-flash rust agent, 1-5 parts of corrosion inhibitor, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of hydrated aluminum magnesium silicate.
6. The titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 1, wherein the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is an oily paint comprising a component A and a component B;
the component A comprises the following raw materials in parts by weight:
10-30 parts of titanium-based polymer alloy copolymer, 8-15 parts of active diluent, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-20 parts of toughening wear-resistant material, 5-15 parts of pigment and filler and 3-8 parts of coating additive;
the imide resin is bismaleimide resin, and the titanium-based polymer alloy copolymer is titanium-based bismaleimide polymer alloy copolymer;
the active diluent is dicyclooxazole or 3-aminopropyl trihydroxy silane, or a mixture of the dicyclooxazole and the 3-aminopropyl trihydroxy silane in any proportion;
the toughening wear-resistant material is one or more than two of elastic saturated polyester resin, liquid nitrile rubber and liquid fluorosilicone rubber;
the pigment and filler comprises a coloring pigment and/or a filler; the coloring pigment comprises carbon black or titanium dioxide, and the filler comprises mica powder or barium sulfate;
the coating auxiliary agent comprises one or more than two of wetting dispersant, defoamer, flatting agent, thickener and anti-settling agent;
the component B is an isocyanate HDI trimer curing agent, and the mass ratio of the component A to the component B is 4-5: 1.
7. the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 6, wherein when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is an oily primer, the component A comprises the following components in parts by mass:
10-20 parts of titanium-based polymer alloy copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxy silane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of liquid nitrile rubber, 10-20 parts of antirust pigment, 10-15 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organic bentonite; the mass ratio of the component A to the component B is 5: 1; the antirust pigment is phosphate or composite phosphate antirust pigment;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is an oily finish, the component A comprises the following components in parts by mass:
20-30 parts of titanium-based high-molecular alloy copolymer, 4-10 parts of bicyclooxazolidine, 4-10 parts of 3-aminopropyl trihydroxysilane, 5-10 parts of phenoxy resin, 5-10 parts of epoxy phenolic resin, 5-10 parts of benzyl silicone resin, 5-10 parts of elastic saturated polyester resin, 5-10 parts of liquid nitrile rubber, 3-5 parts of carbon black, 5-10 parts of mica powder, 0.5-1.5 parts of wetting dispersant, 0.1-1 part of defoaming agent, 0.1-1 part of flatting agent, 0.5-2 parts of fumed silica and 0.5-2 parts of organobentonite; the mass ratio of the component A to the component B is 4: 1.
8. The preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in claim 3, wherein when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is a water-based primer, the preparation method comprises the following steps:
uniformly mixing titanium-based high-molecular alloy copolymer, fully methylated amino resin, styrene-butadiene rubber emulsion, water-soluble phenolic resin, water-based graphene dispersion slurry, a dispersing agent, an anti-flash rust agent, a corrosion inhibitor, fumed silica, hydrated aluminum magnesium silicate, tetrahydrofuran, N-methyl pyrrolidone, a defoaming agent, a leveling agent and a filling material, grinding, adding a pH regulator, adjusting the pH of the system to 7-9, adding polyphenoxy resin emulsion, phenyl silicone resin emulsion and an anti-rust pigment, and uniformly mixing and dispersing;
when the titanium-based polymer alloy high-temperature-resistant anticorrosive paint is water-based finish paint, the preparation method comprises the following steps:
titanium-based polymer alloy copolymer, water-soluble phenolic resin, fully methylated amino resin, tetrahydrofuran, N-methyl pyrrolidone, aqueous graphene dispersion slurry, carbon black, mica powder, fumed silica, hydrated aluminum magnesium silicate, a defoaming agent, a leveling agent, a dispersing agent, a,α-Grinding the phase nano-alumina after uniformly mixing, adding phenyl silicone resin emulsion, butadiene styrene rubber emulsion and poly phenol-oxygen resin emulsion, and uniformly mixing and dispersing.
9. A preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in any one of claims 4 to 5, characterized by comprising the following steps:
uniformly mixing the titanium-based polymer alloy copolymer, the water-soluble phenolic resin, the aqueous dispersion phenyl silicone resin, the anti-rust pigment, the pigment filler and the coating auxiliary agent, grinding, adding the poly (phenol-oxygen resin) emulsion and the styrene butadiene rubber emulsion, and uniformly mixing and dispersing.
10. A preparation method of the titanium-based polymer alloy high-temperature-resistant anticorrosive paint as claimed in any one of claims 6 to 7, characterized by comprising the following steps:
and uniformly mixing the raw materials in the component A in proportion, grinding, filtering and packaging.
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