CN111303741A - High-film-thickness waterborne polyurethane long-acting anticorrosive paint for wind power and petrochemical equipment and preparation method thereof - Google Patents
High-film-thickness waterborne polyurethane long-acting anticorrosive paint for wind power and petrochemical equipment and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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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
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Abstract
The invention discloses a high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment, and belongs to the technical field of waterborne anticorrosive coatings. According to the invention, the modified graphene oxide and acrylic monomers are respectively subjected to solution polymerization and emulsion polymerization to prepare the graphene oxide/hydroxypropyl dispersoid and the graphene oxide/hydroxypropyl emulsion with the core-shell structure, and the graphene oxide/hydroxypropyl emulsion are taken as film forming substances to prepare the high-film-thickness aqueous double-component polyurethane long-acting anticorrosive coating.
Description
Technical Field
The invention relates to the field of aqueous anticorrosive coatings, in particular to a high-film-thickness aqueous polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment and a preparation method thereof.
Background
The equipment manufacturing industry occupies a special important position in the development of China and is an important support for the economic development of China. Wind power and petrochemical equipment are used as important components of the wind power and petrochemical equipment, the operation environment is severe, and the types of environmental climates facing the wind power and petrochemical equipment mainly comprise: coastal, offshore, desert, gobi, etc. The salt corrosion problem is particularly prominent under the coastal and offshore conditions, and the serious corrosion problem is also brought by the wind and sand corrosion in deserts and gobi, which threatens the normal operation of equipment.
In order to improve the protection capability of the product, the thickness of the coating is increased (the thickness of the composite coating reaches over 240 mu m) at present, but the current waterborne polyurethane products have the phenomenon of thick prickly heat coating, so that the popularization and the application of the product are limited, and the reaction principle is as follows: 2RNCO + H2O→RNHCONHR+CO2×, i.e.: one water molecule reacts with 2 isocyanate groups to evolve carbon dioxide gas, from which it can be seen that a small amount of water can consume a large amount of diisocyanate and produce a large amount of gas. When the paint film is closed, the gas which does not escape in time can jack up the paint film to form miliaria, and the surface effect and the coating performance of the paint film are seriously influenced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a high-film-thickness waterborne polyurethane long-acting anticorrosive paint for wind power and petrochemical equipment and a preparation method thereof, and the technical scheme of the invention is as follows:
the long-acting anticorrosive paint comprises a component A and a component B, wherein the mass ratio of the component A to the component B is (5-7) to 1;
wherein, the component A comprises: according to the weight portion, 20-35 portions of graphene oxide/hydroxypropyl dispersoid, 10-20 portions of graphene oxide/hydroxypropyl emulsion, 5-10 portions of polytetrafluoroethylene wax emulsion, 0.3-0.5 portion of fumed silica, 5-10 portions of titanium dioxide, 5-10 portions of silicon micropowder, 5-8 portions of corrosion-resistant powder, 0.6-0.8 portion of dispersing agent, 0.1-0.3 portion of wetting defoamer, 0.2-0.4 portion of anti-explosion auxiliary agent, 0.3-0.5 portion of rheological auxiliary agent, 2-5 portions of cosolvent and 5-10 portions of deionized water;
wherein, the component B comprises: 60-80 parts of water-based isocyanate curing agent and 20-40 parts of cosolvent by weight.
Further, in a preferred embodiment of the present invention, the mass ratio of the graphene oxide/hydroxypropyl dispersion to the graphene oxide/hydroxypropyl emulsion is (1.5-2):1, the average hydroxyl-OH content is 2-2.5 wt%, and the molar ratio of isocyanate group-NCO to average hydroxyl-OH in the aqueous isocyanate curing agent is (1.3-1.5): 1.
Further, in a preferred embodiment of the present invention, the graphene oxide/hydroxypropyl dispersion is prepared by the following steps:
a. preparing a nuclear monomer mixed solution: taking 5-10 parts by weight of modified graphene oxide, 10-25 parts by weight of methyl methacrylate, 5-20 parts by weight of hydroxyethyl methacrylate, 10-20 parts by weight of butyl methacrylate, 5-20 parts by weight of butyl acrylate, 5-15 parts by weight of styrene, 0.5-5 parts by weight of an initiator and 0.5-5 parts by weight of chain transfer;
b. preparing shell monomer mixed solution: taking 5-10 parts by weight of modified graphene oxide, 10-25 parts by weight of methyl methacrylate, 5-20 parts by weight of hydroxyethyl methacrylate, 1-5 parts by weight of methacrylic acid, 10-20 parts by weight of butyl methacrylate, 5-20 parts by weight of butyl acrylate, 5-15 parts by weight of styrene, 0.5-5 parts by weight of an initiator and 0.5-5 parts by weight of chain transfer;
c. preparing graphene oxide/hydroxypropyl dispersion: adding 5-10 parts of dipropylene glycol butyl ether into a four-neck flask provided with a stirrer, a condenser, a thermometer and a constant-pressure dropping funnel, and introducing nitrogen for 15-30min to replace air; when the temperature is raised to 135-140 ℃, 50-80 parts of nuclear monomer mixed solution is dripped, the reaction is dripped at constant speed for 3-4h, and the temperature is kept for 0.5 h; then, dripping 10-20 parts of shell monomer mixed solution, dripping at constant speed for reaction for 1.5-2h, and keeping the temperature for 1 h; and cooling to 100 ℃, adding 0.5-1 part of neutralizing agent, stirring for 0.5h, adding deionized water, dispersing for 0.5-1h, filtering and discharging to obtain the graphene oxide/hydroxypropyl dispersoid.
Further, in a preferred embodiment of the present invention, the chain transfer agent is one of dodecyl mercaptan, AMSD, and isooctyl 3-mercaptopropionate; the neutralizer is one or the combination of N, N-dimethylethanolamine and triethanolamine; the content of hydroxyl in the graphene oxide/hydroxypropyl dispersoid is 3.2-3.5%, and the solid content is 43-46%.
Further, in a preferred embodiment of the present invention, the graphene oxide/hydroxypropyl emulsion is prepared by the following steps:
a. preparation of the core pre-emulsion: dispersing 1-2 parts by weight of anionic emulsifier AS-801, 0.1-0.5 part by weight of nonionic emulsifier X-405 and 20-25 parts by weight of distilled water at high speed for 3-5min, then adding 50-65 parts by weight of methyl methacrylate, 12-20 parts by weight of styrene, 5-10 parts by weight of hydroxyethyl ester, 1.5-2 parts by weight of acrylic acid, 3 parts by weight of AGE, 2-5 parts by weight of butyl acrylate, 1.5 parts by weight of DPM and 3-10 parts by weight of modified graphene oxide, stirring at high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 parts by weight of initiator aqueous solution, and dispersing uniformly to obtain a core pre-emulsion;
b. preparation of the shell pre-emulsion: dispersing 1-2 parts by weight of AS-801, 0.1-0.5 part by weight of X-405 and 20-25 parts by weight of distilled water at a high speed for 3-5min, then adding 50-65 parts by weight of methyl methacrylate, 14-20 parts by weight of styrene, 5-10 parts by weight of hydroxyethyl ester, 0.5 part by weight of TMPTA, 5.5 parts by weight of IBOA, 1.5-2 parts by weight of acrylic acid, 0.25 part by weight of benzoyl peroxide, 1.5 parts by weight of DPM and 3-10 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 initiator aqueous solution, and dispersing uniformly to obtain a shell pre-emulsion;
c. preparing graphene oxide/hydroxypropyl emulsion: adding 1-2 parts by weight of AS-801, 0.1-0.5 part by weight of X-405, 0.15-0.2 part by weight of sodium bicarbonate and 0.3-0.5 part by weight of alcohol ester twelve and 20-25 parts by weight of distilled water into a four-neck flask provided with a stirrer, a condenser tube, a thermometer and a constant pressure dropping funnel, stirring, emulsifying, heating to 82-83 ℃, adding 1/4 of nuclear pre-emulsion, adding 1/5 of initiator aqueous solution, and reacting for 0.5h after blue light appears; heating to 88-90 deg.c and dropping the rest pre-emulsion; dropping the shell pre-emulsion at 88-90 ℃, keeping the total dropping time for 6.5-7 h, keeping the temperature for 1.5h after dropping, then raising the temperature to 90-92 ℃, keeping the temperature for 1h, cooling to below 60 ℃, discharging to obtain graphene oxide/hydroxypropyl emulsion;
wherein the initiator aqueous solution is 0.2-0.4 part of ammonium persulfate dissolved by 0.4-0.6 part of distilled water.
Further, in a preferred embodiment of the present invention, the mass ratio of the core pre-emulsion to the shell pre-emulsion is 8: 92;
the content of hydroxyl in the graphene oxide/hydroxypropyl emulsion is 1.4-1.6%, and the solid content is 42-45%.
Further, in a preferred embodiment of the present invention, the modified graphene oxide is prepared by graft-modifying the surface of graphene oxide with styryl trimethoxysilane.
Further, in a preferred embodiment of the present invention, the modified graphene oxide has the following structural formula:
further, in a preferred embodiment of the present invention, the corrosion-resistant powder is one or a combination of phosphate and zinc salt of organic nitrogen compound; the dispersant is one or more of organic high molecular polymers, polyvalent carboxylic acids and silicates; the wetting defoaming agent is one or the combination of surfynol 104E and DYNOL 604 of surfactant with acetylene glycol gemini structure; the anti-foaming auxiliary agent is one or the combination of BYKETOL-LP and BYKETOL-AQ; the rheological additive is polyurethane tackifier; the cosolvent is one or the combination of oxygen acid ester environment-friendly solvent PCC and water-oil amphoteric non-VOC environment-friendly odorless solvent 2-methyl-2, 4-pentanediol MPD.
The preparation method of the high-film-thickness waterborne polyurethane long-acting anticorrosive paint for wind power and petrochemical equipment comprises the following steps of:
(1) preparation of component A:
uniformly mixing the graphene oxide/hydroxypropyl dispersoid, 2/3 deionized water, a dispersing agent, a wetting defoaming agent, an anti-foaming auxiliary agent, polytetrafluoroethylene wax emulsion, fumed silica, titanium dioxide, silicon micropowder, corrosion-resistant powder and a cosolvent according to a proportion, grinding the mixture to the fineness of 20 microns, adding the graphene oxide/hydroxypropyl emulsion and the rest deionized water, uniformly mixing the mixture, adding a rheological auxiliary agent, and adjusting the viscosity to 80KU to prepare a component A;
(2) preparation of the component B: and uniformly mixing the water-based isocyanate curing agent and the cosolvent according to a proportion to prepare the component B.
The invention has the beneficial effects that:
the invention fully combines the characteristics of high hardness and high chemical resistance of the high-hydroxyl acrylic acid dispersoid, large molecular weight of the low-hydroxyl acrylic acid emulsion, certain mechanical strength of the low-hydroxyl acrylic acid emulsion and less consumption of the needed isocyanate curing agent, compounds the high-hydroxyl acrylic acid dispersoid and the low-hydroxyl acrylic acid emulsion, prolongs the open time of a paint film by using a high-boiling-point solvent, simultaneously improves the solid content of the paint and reduces the specific gravity of water, preferentially selects a wetting agent and an anti-bubble auxiliary agent with defoaming function, reserves time for residual bubbles and reactive gas to escape from the paint film, ensures that the bubbles escape before the paint film is sealed, and effectively avoids the problem of miliaria caused by a high-film-thickness coating through the measures.
According to the invention, the styryl trimethoxy silane is anchored on the surface of Graphene Oxide (GO) and is subjected to in-situ polymerization with an acrylic monomer, so that a polymer grows on the graphene, the graphene is promoted to be uniformly dispersed in a coating, and better corrosion resistance and wear resistance are shown.
According to the invention, the film-forming resin with high and low hydroxyl content is compounded as a film-forming substance of the coating, the weight ratio of hydroxypropyl dispersoid to hydroxypropyl emulsion is 1.5-2: 1, the average hydroxyl content is controlled to be 2-2.5 wt%, the NCO/OH range is 1.3-1.5, the miliaria problem of the coating with high film thickness is effectively avoided by preferably selecting the reasonable proportion of hydroxypropyl dispersoid to hydroxypropyl emulsion, controlling the average hydroxyl content, the reaction group ratio and other measures, and meanwhile, the coating has the characteristics of excellent acid and alkali resistance, corrosion resistance, wear resistance and the like.
The high-film-thickness waterborne polyurethane long-acting anticorrosive coating provided by the invention has the advantages that the thickness of a one-time spraying wet film is more than 200 mu m, the thickness of a dry film is more than 110 mu m, no dark bubbles or miliaria are generated on the surface of the paint film, and the popularization and the application of the waterborne polyurethane coating are facilitated.
Drawings
FIG. 1 is a photograph showing a salt spray test of an anticorrosive coating according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 5: 1.
The component A comprises: calculated by weight parts, 20 parts of graphene oxide/hydroxypropyl dispersoid, 20 parts of graphene oxide/hydroxypropyl emulsion, 10 parts of polytetrafluoroethylene wax emulsion, 0.5 part of fumed silica, 10 parts of titanium dioxide, 10 parts of silicon micropowder, 8 parts of corrosion-resistant powder, 0.6 part of dispersing agent, 0.3 part of wetting defoaming agent, 0.2 part of anti-foaming auxiliary agent, 0.3 part of rheological auxiliary agent, 2 parts of cosolvent and 18 parts of deionized water. The component B comprises: 80 parts of water-based isocyanate curing agent and 20 parts of cosolvent by weight.
In this example, the mass ratio of the graphene oxide/hydroxypropyl dispersion to the graphene oxide/hydroxypropyl emulsion is 1.5:1, the average hydroxyl content is 2.5 wt%, and the NCO/OH ratio is 1.3: 1.
The graphene oxide/hydroxypropyl dispersion of this example was prepared by the following steps:
a. preparing a nuclear monomer mixed solution: taking 5 parts by weight of modified graphene oxide, 24 parts by weight of methyl methacrylate, 20 parts by weight of hydroxyethyl methacrylate, 20 parts by weight of butyl methacrylate, 15 parts by weight of butyl acrylate, 15 parts by weight of styrene, 0.5 part by weight of an initiator and 0.5 part by weight of chain transfer;
b. preparing shell monomer mixed solution: taking 5 parts by weight of modified graphene oxide, 24 parts by weight of methyl methacrylate, 15 parts by weight of hydroxyethyl methacrylate, 5 parts by weight of methacrylic acid, 20 parts by weight of butyl methacrylate, 15 parts by weight of butyl acrylate, 5 parts by weight of styrene, 0.5 part by weight of initiator and 0.5 part by weight of chain transfer;
c. preparing graphene oxide/hydroxypropyl dispersion: adding 5 parts of dipropylene glycol butyl ether into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a constant-pressure dropping funnel, and introducing nitrogen for 15min to replace air; when the temperature is raised to 135 ℃, 80 parts of nuclear monomer mixed solution is dripped, the reaction is carried out for 3 hours at a constant speed, and the temperature is kept for 0.5 hour; then, 16 parts of shell monomer mixed solution is dripped, the mixture is dripped at constant speed for reaction for 1.5h, and the temperature is kept for 1 h; and cooling to 100 ℃, adding 0.5 part of neutralizing agent, stirring for 0.5h, adding deionized water, dispersing for 0.5h, filtering and discharging to obtain the graphene oxide/hydroxypropyl dispersoid. The hydroxyl content of the graphene oxide/hydroxypropyl dispersion is 3.2%, and the solid content is 43%.
The graphene oxide/hydroxypropyl emulsion of the present embodiment is prepared by the following steps:
a. preparation of the core pre-emulsion: dispersing 1 part by weight of AS-801, 0.1 part by weight of X-405 and 25 parts by weight of distilled water at a high speed for 3-5min, then adding 50 parts by weight of methyl methacrylate, 20 parts by weight of styrene, 10 parts by weight of hydroxyethyl ester, 2 parts by weight of acrylic acid, 3 parts by weight of AGE, 5 parts by weight of butyl acrylate, 1.5 parts by weight of DPM and 8.5 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 of initiator aqueous solution, and dispersing uniformly to obtain a core pre-emulsion;
b. preparation of the shell pre-emulsion: dispersing 2 parts by weight of AS-801, 0.5 part by weight of X-405 and 25 parts by weight of distilled water at a high speed for 3-5min, then adding 65 parts by weight of methyl methacrylate, 14 parts by weight of styrene, 10 parts by weight of hydroxyethyl ester, 0.5 part by weight of TMPTA, 5.5 parts by weight of IBOA, 2 parts by weight of acrylic acid, 0.25 part by weight of benzoyl peroxide, 1.5 parts by weight of DPM and 3 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 initiator aqueous solution, and dispersing uniformly to obtain shell pre-emulsion;
c. preparing graphene oxide/hydroxypropyl emulsion: adding 2 parts by weight of AS-801, 0.5 part by weight of X-405, 0.15 part by weight of sodium bicarbonate, 0.3 part by weight of alcohol ester twelve and 20 parts by weight of distilled water into a four-neck flask provided with a stirrer, a condenser, a thermometer and a constant pressure dropping funnel, stirring, emulsifying, heating to 82 ℃, adding 1/4 parts of nuclear pre-emulsion, adding 1/5 parts of initiator aqueous solution, and reacting for 0.5 hour after blue light appears; heating to 88-90 deg.c and dropping the rest pre-emulsion; dropping the shell pre-emulsion at 88-90 ℃, keeping the total dropping time for 6.5h, keeping the temperature for 1.5h after dropping, then raising the temperature to 90 ℃, keeping the temperature for 1h, cooling to below 60 ℃, discharging, and obtaining the graphene oxide/hydroxypropyl emulsion.
Wherein the initiator aqueous solution is 0.2 part of ammonium persulfate and 0.4 part of distilled water
The mass ratio of the core pre-emulsion to the shell pre-emulsion was 8: 92. The hydroxyl content of the graphene oxide/hydroxypropyl emulsion is 1.4%, and the solid content is 42%.
The modified graphene oxide of the embodiment is prepared by grafting and modifying the surface of graphene oxide with styryl trimethoxy silane, and the synthetic reaction formula is as follows:
the modified graphene oxide has the following structural formula:
the specific steps for preparing the modified graphene oxide are as follows:
0.1 part of graphene oxide and 100 parts of 10% NMP aqueous solution are uniformly mixed, ultrasonically dispersed for 2 hours, the pH of the mixed solution is adjusted to 3 by hydrochloric acid, styryl trimethoxy silane is added, the mixed solution is slowly heated to 80 ℃, and is subjected to constant-temperature reaction for 3 hours under the conditions of acid and heating, cooled, washed by isopropanol and water, and dried to obtain the modified graphene oxide.
The preparation method of the high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment comprises the following steps of:
(1) preparation of component A: uniformly mixing the graphene oxide/hydroxypropyl dispersoid, 2/3 deionized water, a dispersing agent, a wetting defoaming agent, an anti-foaming auxiliary agent, polytetrafluoroethylene wax emulsion, fumed silica, titanium dioxide, silicon micropowder, corrosion-resistant powder and a cosolvent according to a proportion, grinding the mixture to the fineness of 20 microns, adding the graphene oxide/hydroxypropyl emulsion and the rest deionized water, uniformly mixing the mixture, adding a rheological auxiliary agent, and adjusting the viscosity to 80KU to prepare a component A;
(2) preparation of the component B: and uniformly mixing the water-based isocyanate curing agent and the cosolvent according to a proportion to prepare the component B.
In this embodiment: the chain transfer agent is dodecyl mercaptan. The neutralizer is N, N-dimethylethanolamine. The corrosion-resistant powder is phosphate. The dispersant is organic high molecular polymer. The wetting defoaming agent is a surfactant surfynol 104E with an acetylene glycol gemini structure. The anti-foaming auxiliary agent is BYKETOL-LP. The rheological additive is polyurethane tackifier. The cosolvent is oxygen acid ester environment-friendly solvent PCC.
Example 2
The high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 7: 1.
The component A comprises: calculated by weight parts, 35 parts of graphene oxide/hydroxypropyl dispersoid, 15 parts of graphene oxide/hydroxypropyl emulsion, 5 parts of polytetrafluoroethylene wax emulsion, 0.3 part of fumed silica, 16 parts of titanium dioxide, 15 parts of silicon micropowder, 5 parts of corrosion-resistant powder, 0.6 part of dispersing agent, 0.3 part of wetting defoaming agent, 0.2 part of anti-foaming auxiliary agent, 0.3 part of rheological auxiliary agent, 2 parts of cosolvent and 5.5 parts of deionized water. The component B comprises: 70 parts of water-based isocyanate curing agent and 30 parts of cosolvent by weight.
In this example, the mass ratio of the graphene oxide/hydroxypropyl dispersion to the graphene oxide/hydroxypropyl emulsion is 2:1, the average hydroxyl content is 2.5 wt%, and the NCO/OH ratio is 1.5: 1.
The graphene oxide/hydroxypropyl dispersion of this example was prepared by the following steps:
a. preparing a nuclear monomer mixed solution: taking 8 parts by weight of modified graphene oxide, 21 parts by weight of methyl methacrylate, 20 parts by weight of hydroxyethyl methacrylate, 20 parts by weight of butyl methacrylate, 15 parts by weight of butyl acrylate, 15 parts by weight of styrene, 0.5 part by weight of an initiator and 0.5 part by weight of chain transfer;
b. preparing shell monomer mixed solution: taking 8 parts by weight of modified graphene oxide, 21 parts by weight of methyl methacrylate, 15 parts by weight of hydroxyethyl methacrylate, 5 parts by weight of methacrylic acid, 20 parts by weight of butyl methacrylate, 15 parts by weight of butyl acrylate, 15 parts by weight of styrene, 0.5 part by weight of initiator and 0.5 part by weight of chain transfer agent;
c. preparing graphene oxide/hydroxypropyl dispersion: adding 5 parts of dipropylene glycol butyl ether into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a constant-pressure dropping funnel, and introducing nitrogen for 15min to replace air; when the temperature is raised to 135 ℃, 75 parts of nuclear monomer mixed solution is dripped, the reaction is dripped at constant speed for 4 hours, and the temperature is kept for 0.5 hour; then, 15 parts of shell monomer mixed solution is dripped, the mixture is dripped at a constant speed for reaction for 2 hours, and the temperature is kept for 1 hour; and cooling to 100 ℃, adding 0.5 part of neutralizing agent, stirring for 0.5h, adding deionized water, dispersing for 0.5h, filtering and discharging to obtain the graphene oxide/hydroxypropyl dispersoid. The hydroxyl content of the graphene oxide/hydroxypropyl dispersion was 3.5%, and the solids content was 46%.
The graphene oxide/hydroxypropyl emulsion of the present embodiment is prepared by the following steps:
a. preparation of the core pre-emulsion: dispersing 2 parts by weight of AS-801, 0.5 part by weight of X-405 and 20 parts by weight of distilled water at a high speed for 3-5min, then adding 65 parts by weight of methyl methacrylate, 12 parts by weight of styrene, 5 parts by weight of hydroxyethyl ester, 1.5 parts by weight of acrylic acid, 3 parts by weight of AGE, 2 parts by weight of butyl acrylate, 1.5 parts by weight of DPM and 10 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 of initiator aqueous solution, and dispersing uniformly to obtain a core pre-emulsion;
b. preparation of the shell pre-emulsion: dispersing 1 part by weight of AS-801, 0.1 part by weight of X-405 and 20 parts by weight of distilled water at a high speed for 3-5min, then adding 58 parts by weight of methyl methacrylate, 20 parts by weight of styrene, 5 parts by weight of hydroxyethyl ester, 0.5 part by weight of TMPTA, 5.5 parts by weight of IBOA, 1.5 parts by weight of acrylic acid, 0.25 part by weight of benzoyl peroxide, 1.5 parts by weight of DPM and 8 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 initiator aqueous solution, and dispersing uniformly to obtain shell pre-emulsion;
c. preparing graphene oxide/hydroxypropyl emulsion: adding 1.5 parts by weight of AS-801, 0.35 part by weight of X-405, 0.2 part by weight of sodium bicarbonate, 0.4 part by weight of alcohol ester dodeca and 25 parts by weight of distilled water into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a constant pressure dropping funnel, stirring, emulsifying, heating to 83 ℃, adding 1/4 parts of nuclear pre-emulsion, adding 1/5 parts of initiator aqueous solution, and reacting for 0.5 hour after blue light appears; heating to 90 ℃, and dropwise adding the rest of the nuclear pre-emulsion; dropping the shell pre-emulsion at 90 ℃, keeping the total dropping time for 7h, keeping the temperature for 1.5h after dropping, then heating to 92 ℃ and keeping the temperature for 1h, then cooling to below 60 ℃, and discharging to obtain the graphene oxide/hydroxypropyl emulsion.
Wherein the initiator aqueous solution is 0.4 part of ammonium persulfate dissolved by 0.6 part of distilled water
The mass ratio of the core pre-emulsion to the shell pre-emulsion was 8: 92. The hydroxyl content of the graphene oxide/hydroxypropyl emulsion is 1.6%, and the solid content is 45%.
The specific steps for preparing the modified graphene oxide in this embodiment are as follows:
0.3 part of graphene oxide and 100 parts of 10% NMP aqueous solution are uniformly mixed, ultrasonically dispersed for 3 hours, the pH of the mixed solution is adjusted to 3-4 by hydrochloric acid, styryl trimethoxy silane is added, the mixed solution is slowly heated to 80 ℃, the mixed solution is subjected to constant temperature reaction for 5 hours under the conditions of acid and heating, cooled, washed by isopropanol and water, and dried to obtain the modified graphene oxide.
The preparation method of the high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment comprises the following steps of:
(1) preparation of component A: uniformly mixing the graphene oxide/hydroxypropyl dispersoid, 2/3 deionized water, a dispersing agent, a wetting defoaming agent, an anti-foaming auxiliary agent, polytetrafluoroethylene wax emulsion, fumed silica, titanium dioxide, silicon micropowder, corrosion-resistant powder and a cosolvent according to a proportion, grinding the mixture to the fineness of 20 microns, adding the graphene oxide/hydroxypropyl emulsion and the rest deionized water, uniformly mixing the mixture, adding a rheological auxiliary agent, and adjusting the viscosity to 80KU to prepare a component A;
(2) preparation of the component B: and uniformly mixing the water-based isocyanate curing agent and the cosolvent according to a proportion to prepare the component B.
In this embodiment: the chain transfer agent is isooctyl 3-mercaptopropionate. The neutralizer is triethanolamine. The corrosion-resistant powder is zinc salt of organic nitrogen compound. The dispersant is a polyvalent carboxylic acid. The wetting defoamer was DYNOL 604. The anti-foaming auxiliary agent is BYKETOL-AQ. The rheological additive is polyurethane tackifier. The cosolvent is a water-oil amphiprotic non-VOC environment-friendly odorless solvent 2-methyl-2, 4-pentanediol MPD.
Example 3
The high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment comprises a component A and a component B, wherein the mass ratio of the component A to the component B is 6: 1. the preparation method comprises the following steps:
(1) preparation of component A: uniformly mixing 30 parts of graphene oxide/hydroxypropyl dispersoid, 8 parts of deionized water, 0.6 part of dispersing agent, 0.3 part of wetting defoaming agent, 0.2 part of anti-foaming auxiliary agent, 10 parts of polytetrafluoroethylene wax emulsion, 0.5 part of fumed silica, 14 parts of titanium dioxide, 12 parts of silicon micropowder, 8 parts of corrosion-resistant powder and 3 parts of cosolvent, grinding the mixture to the fineness of 20 microns, adding 15 parts of graphene oxide/hydroxypropyl emulsion and the rest of deionized water, uniformly mixing, adding 0.3 part of rheological auxiliary agent, and adjusting the viscosity to 80KU to prepare a component A;
(2) preparation of the component B: and (3) uniformly mixing 60 parts of water-based isocyanate curing agent and 40 parts of cosolvent to prepare the component B.
The graphene oxide/hydroxypropyl dispersion of example 1 and the graphene oxide/hydroxypropyl emulsion of example 2 were cited for the coating preparation of example 3.
In this example, the mass ratio of the graphene oxide/hydroxypropyl dispersion to the graphene oxide/hydroxypropyl emulsion is 1.8:1, the average hydroxyl content is 2.2 wt%, and the NCO/OH ratio is 1.4: 1.
In this embodiment: the neutralizer is N, N-dimethylethanolamine. The corrosion-resistant powder is a combination of phosphate and zinc salt of an organic nitrogen compound. The dispersant is silicate. The wetting defoamer was DYNOL 604. The anti-foaming auxiliary agent is a combination of BYKETOL-LP and BYKETOL-AQ. The rheological additive is polyurethane tackifier. The cosolvent is oxygen acid ester environment-friendly solvent PCC.
Comparative example
Preparation of hydroxypropyl dispersion of this comparative example:
a. nuclear monomer mixed solution: 25 parts of methyl methacrylate, 20 parts of hydroxyethyl methacrylate, 20 parts of butyl methacrylate, 19 parts of butyl acrylate, 14 parts of styrene, 0.5 part of initiator and 0.5 part of chain transfer.
b. Shell monomer mixed solution: 25 parts of methyl methacrylate, 15 parts of hydroxyethyl methacrylate, 5 parts of methacrylic acid, 20 parts of butyl methacrylate, 19 parts of butyl acrylate, 14 parts of styrene, 0.5 part of an initiator and 0.5 part of chain transfer.
c. Adding 5 parts of dipropylene glycol butyl ether into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a constant-pressure dropping funnel, introducing nitrogen for 20min to displace air, heating to 135 ℃, starting to dropwise add 80 parts of core monomer mixed solution, dropwise adding at a constant speed for reaction for 4h, preserving heat for 0.5h, dropwise adding 16 parts of shell monomer mixed solution, dropwise adding at a constant speed for reaction for 3h, preserving heat for 1h, cooling to 100 ℃, adding 0.5 part of neutralizer for stirring for 0.5h, adding deionized water for dispersing for 0.5h, filtering and discharging to obtain the milky white hydroxypropyl dispersion with blue light and having a core-shell structure.
The preparation method of the waterborne polyurethane anticorrosive paint comprises the following steps:
preparation of component A: uniformly mixing 45 parts of hydroxypropyl dispersoid, 8 parts of deionized water, 0.6 part of dispersing agent, 0.3 part of wetting defoaming agent, 0.2 part of anti-foaming auxiliary agent, 10 parts of polytetrafluoroethylene wax emulsion, 0.5 part of fumed silica, 14 parts of titanium dioxide, 12 parts of silica powder, 8 parts of corrosion-resistant powder and 3 parts of cosolvent, grinding to the fineness of 20 microns, adding the rest deionized water, uniformly mixing, adding 0.3 part of rheological auxiliary agent, and adjusting the viscosity to 80KU by using a stormer viscometer to obtain a component A;
preparation of the component B: and uniformly mixing 70 parts of water-based isocyanate curing agent and 30 parts of cosolvent.
The mass ratio of the component A to the component B of the comparative example was 6: 1.
Examples of the experiments
In order to demonstrate the technical effects of the technical solution of the present invention, the coatings prepared in examples 1 to 3 and comparative example were subjected to the performance measurement, and the measurement results are shown in the following table 1:
table 1 aqueous anti-corrosive coatings test data
In addition, the anticorrosive paint of the embodiment of the invention is coated on the surface of a sample to carry out a neutral salt spray test, which is detected by a Youlhongxin detection company, fig. 1 shows the test process, the equipment used in the test is a salt spray test box with the model of GT-041, and the laboratory environment is as follows: 22.4 ℃ and 51% RH. The test conditions included: the reference standard is GB/T1771-2007, the size of the sample is 150mm multiplied by 100mm, the test time is 6000h, and the test results are shown in Table 2.
TABLE 2 salt spray test results
From the results, the thickness of the dry film in the examples 1 to 3 is 110 to 120 μm, no dark bubbles or miliaria are generated on the surface of the paint film, the wear resistance is less than 40mg, the neutral salt fog resistance is more than 6000h, and the coating has the characteristics of excellent mechanics, aging resistance, acid and alkali salt resistance and the like.
In conclusion, the modified graphene oxide and the acrylic monomer are respectively subjected to solution polymerization and emulsion polymerization to prepare the graphene oxide/hydroxypropyl dispersion and the graphene oxide/hydroxypropyl emulsion with the core-shell structure, and the graphene oxide/hydroxypropyl dispersion and the graphene oxide/hydroxypropyl emulsion are used as film forming substances, so that the long-acting anticorrosive coating of the high-film-thickness and high-wear-resistance aqueous graphene polyurethane can be obtained.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (10)
1. The long-acting anticorrosive coating is characterized by comprising a component A and a component B, wherein the mass ratio of the component A to the component B is (5-7) to 1;
wherein, the component A comprises: according to the weight portion, 20-35 portions of graphene oxide/hydroxypropyl dispersoid, 10-20 portions of graphene oxide/hydroxypropyl emulsion, 5-10 portions of polytetrafluoroethylene wax emulsion, 0.3-0.5 portion of fumed silica, 5-10 portions of titanium dioxide, 5-10 portions of silicon micropowder, 5-8 portions of corrosion-resistant powder, 0.6-0.8 portion of dispersing agent, 0.1-0.3 portion of wetting defoamer, 0.2-0.4 portion of anti-explosion auxiliary agent, 0.3-0.5 portion of rheological auxiliary agent, 2-5 portions of cosolvent and 5-10 portions of deionized water;
wherein, the component B comprises: 60-80 parts of water-based isocyanate curing agent and 20-40 parts of cosolvent by weight.
2. The long-acting anticorrosive coating of high-film-thickness aqueous polyurethane for wind power and petrochemical equipment according to claim 1, wherein the mass ratio of the graphene oxide/hydroxypropyl dispersion to the graphene oxide/hydroxypropyl emulsion is (1.5-2):1, the average hydroxyl-OH content is 2-2.5 wt%, and the molar ratio of isocyanate-NCO to the average hydroxyl-OH in the aqueous isocyanate curing agent is (1.3-1.5): 1.
3. The high-film-thickness aqueous polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment according to claim 1 or 2, wherein the graphene oxide/hydroxypropyl dispersion is prepared by the following steps:
a. preparing a nuclear monomer mixed solution: taking 5-10 parts by weight of modified graphene oxide, 10-25 parts by weight of methyl methacrylate, 5-20 parts by weight of hydroxyethyl methacrylate, 10-20 parts by weight of butyl methacrylate, 5-20 parts by weight of butyl acrylate, 5-15 parts by weight of styrene, 0.5-5 parts by weight of an initiator and 0.5-5 parts by weight of chain transfer;
b. preparing shell monomer mixed solution: taking 5-10 parts by weight of modified graphene oxide, 10-25 parts by weight of methyl methacrylate, 5-20 parts by weight of hydroxyethyl methacrylate, 1-5 parts by weight of methacrylic acid, 10-20 parts by weight of butyl methacrylate, 5-20 parts by weight of butyl acrylate, 5-15 parts by weight of styrene, 0.5-5 parts by weight of an initiator and 0.5-5 parts by weight of chain transfer;
c. preparing graphene oxide/hydroxypropyl dispersion: adding 5-10 parts of dipropylene glycol butyl ether into a four-neck flask provided with a stirrer, a condenser, a thermometer and a constant-pressure dropping funnel, and introducing nitrogen for 15-30min to replace air; when the temperature is raised to 135-140 ℃, 50-80 parts of the nuclear monomer mixed solution is dripped, the reaction is dripped at constant speed for 3-4h, and the temperature is kept for 0.5 h; then, dripping 10-20 parts of shell monomer mixed solution, dripping at constant speed for reaction for 1.5-2h, and preserving heat for 1 h; and cooling to 100 ℃, adding 0.5-1 part of neutralizing agent, stirring for 0.5h, adding deionized water, dispersing for 0.5-1h, filtering and discharging to obtain the graphene oxide/hydroxypropyl dispersoid.
4. The long-acting anticorrosive coating of high-film-thickness aqueous polyurethane for wind power and petrochemical equipment according to claim 3, characterized in that,
the chain transfer agent is one of dodecyl mercaptan, AMSD and 3-isooctyl mercaptopropionate;
the neutralizing agent is one or the combination of N, N-dimethylethanolamine and triethanolamine;
the content of hydroxyl in the graphene oxide/hydroxypropyl dispersoid is 3.2-3.5%, and the solid content is 43-46%.
5. The high-film-thickness waterborne polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment according to claim 1 or 2, wherein the graphene oxide/hydroxypropyl emulsion is prepared by the following steps:
a. preparation of the core pre-emulsion: dispersing 1-2 parts by weight of anionic emulsifier AS-801, 0.1-0.5 part by weight of nonionic emulsifier X-405 and 20-25 parts by weight of distilled water at high speed for 3-5min, then adding 50-65 parts by weight of methyl methacrylate, 12-20 parts by weight of styrene, 5-10 parts by weight of hydroxyethyl ester, 1.5-2 parts by weight of acrylic acid, 3 parts by weight of AGE, 2-5 parts by weight of butyl acrylate, 1.5 parts by weight of DPM and 3-10 parts by weight of modified graphene oxide, stirring at high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 parts by weight of initiator aqueous solution, and dispersing uniformly to obtain a core pre-emulsion;
b. preparation of the shell pre-emulsion: dispersing 1-2 parts by weight of AS-801, 0.1-0.5 part by weight of X-405 and 20-25 parts by weight of distilled water at a high speed for 3-5min, then adding 50-65 parts by weight of methyl methacrylate, 14-20 parts by weight of styrene, 5-10 parts by weight of hydroxyethyl ester, 0.5 part by weight of TMPTA, 5.5 parts by weight of IBOA, 1.5-2 parts by weight of acrylic acid, 0.25 part by weight of benzoyl peroxide, 1.5 parts by weight of DPM and 3-10 parts by weight of modified graphene oxide, stirring at a high speed for 0.5h at room temperature to completely emulsify, then adding 2/5 initiator aqueous solution, and dispersing uniformly to obtain a shell pre-emulsion;
c. preparing graphene oxide/hydroxypropyl emulsion: adding 1-2 parts by weight of AS-801, 0.1-0.5 part by weight of X-405, 0.15-0.2 part by weight of sodium bicarbonate and 0.3-0.5 part by weight of alcohol ester twelve and 20-25 parts by weight of distilled water into a four-neck flask provided with a stirrer, a condenser tube, a thermometer and a constant pressure dropping funnel, stirring, emulsifying, heating to 82-83 ℃, adding 1/4 of nuclear pre-emulsion, adding 1/5 of initiator aqueous solution, and reacting for 0.5h after blue light appears; heating to 88-90 deg.c and dropping the rest pre-emulsion; dropping the shell pre-emulsion at 88-90 ℃, keeping the total dropping time for 6.5-7 h, keeping the temperature for 1.5h after dropping, then raising the temperature to 90-92 ℃, keeping the temperature for 1h, cooling to below 60 ℃, discharging to obtain graphene oxide/hydroxypropyl emulsion;
wherein the initiator aqueous solution is 0.2-0.4 part of ammonium persulfate dissolved by 0.4-0.6 part of distilled water.
6. The long-acting anticorrosive coating of high-film-thickness aqueous polyurethane for wind power and petrochemical equipment according to claim 5,
the mass ratio of the core pre-emulsion to the shell pre-emulsion is 8: 92;
the hydroxyl content of the graphene oxide/hydroxypropyl emulsion is 1.4-1.6%, and the solid content is 42-45%.
7. The long-acting anticorrosive coating of high-film-thickness waterborne polyurethane for wind power and petrochemical equipment according to claim 4 or 6, wherein the modified graphene oxide is prepared by grafting and modifying the surface of graphene oxide with styryl trimethoxy silane.
8. The high-film-thickness aqueous polyurethane long-acting anticorrosive coating for wind power and petrochemical equipment according to claim 7, wherein the modified graphene oxide has the following structural formula:
9. the long-acting anticorrosive coating of high-film-thickness aqueous polyurethane for wind power and petrochemical equipment according to claim 1, characterized in that,
the corrosion-resistant powder is one or the combination of phosphate and organic nitrogen compound zinc salt;
the dispersant is one or more of organic high molecular polymers, multivalent carboxylic acids and silicates;
the wetting defoaming agent is one or the combination of surfynol 104E and DYNOL 604 of surfactants with acetylene glycol gemini structures;
the anti-foaming auxiliary agent is one or a combination of BYKETOL-LP and BYKETOL-AQ;
the rheological additive is a polyurethane tackifier;
the cosolvent is one or the combination of oxygen acid ester environment-friendly PCC as an environment-friendly solvent and a water-oil amphoteric non-VOC environment-friendly odorless solvent 2-methyl-2, 4-pentanediol MPD.
10. The preparation method of the high-film-thickness aqueous polyurethane long-acting anticorrosive paint for wind power and petrochemical equipment according to any one of claims 1 to 9, characterized by comprising the following steps:
(1) preparation of component A:
uniformly mixing the graphene oxide/hydroxypropyl dispersoid, 2/3 deionized water, a dispersing agent, a wetting defoaming agent, an anti-foaming auxiliary agent, polytetrafluoroethylene wax emulsion, fumed silica, titanium dioxide, silicon micropowder, corrosion-resistant powder and a cosolvent according to the proportion, grinding the mixture to the fineness of 20 microns, adding the graphene oxide/hydroxypropyl emulsion and the rest deionized water, uniformly mixing the mixture, adding a rheological auxiliary agent, and adjusting the viscosity to 80KU to prepare a component A;
(2) preparation of the component B: and uniformly mixing the water-based isocyanate curing agent and the cosolvent according to a proportion to prepare the component B.
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