CN109135528B - Water-based antirust sealing agent - Google Patents
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- 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
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a water-based antirust sealing agent, and belongs to the field of metal protection. In the invention, after sodium alginate is dispersed by ultrasonic waves, the o-diol structure of the sodium alginate is changed into a dialdehyde structure under the oxidation of sodium periodate, aldehyde groups in multi-aldehyde sodium alginate can be partially subjected to aldol condensation with active hydroxyl groups in microcrystalline cellulose, and free iron ions are adsorbed and fixed, so that the possibility of corrosion can be effectively reduced; the aluminum powder slurry prepared by taking the aluminum powder as the raw material improves the binding power of the aluminum powder and the polyurethane urea in the composite antirust component A, improves the anticorrosion effect of the closed antirust film, and effectively improves the adhesion, corrosion resistance and other performances after use. The invention solves the problems of poor adhesive force effect and corrosion resistance of the commonly used water-based antirust sealing agent at present.
Description
Technical Field
The invention belongs to the field of metal protection, and particularly relates to a water-based antirust sealing agent.
Background
Before painting, spraying plastics or electroplating, the surface of steel is pretreated by phosphorization and passivation to improve the rust resistance and adhesion of the surface of steel. Manual rust removal or acid pickling rust removal is used in the traditional industry. Manual rust removal, the earliest applied surface treatment method, was used for small area parts and places where sand blasting is not required, and it can remove attached scale, rust products, and loose paint skin and other impurities. At present, the phosphate conversion film treatment is widely applied to products such as automobiles, ships, machinery manufacturing, aerospace, household appliances and the like. The pickling solution of the pickling and rust removing process is generally a mixture of various acids, mainly sulfuric acid, nitric acid, hydrofluoric acid and the like, and the mixed acids have strong corrosivity, strong oxidability and high temperature of corrosive media. The acid pickling rust removal treatment of steel is widely applied to removing the surface iron oxide scales of cold-rolled plate blanks and hot-rolled plates, and the acid pickling is still an indispensable technological process in steel production and steel surface treatment. But also brings about some problems as follows: 1. a large amount of steel materials and acid are consumed. In the pickling process, some iron scales are removed mainly by the chemical reaction of acid and iron scales to dissolve corresponding metal oxides. In some cases, when pickling steel with sulfuric acid, scale is removed by the peeling action of hydrogen bubbles generated by the chemical reaction of the acid with steel. Therefore, a large amount of acid is consumed in the pickling process. Although the use of pickling corrosion inhibitors in pickling can reduce the metal consumption of steel, a considerable amount of metallic iron is lost. 2. The physical properties of the steel may be degraded. During the pickling process, a chemical reaction occurs between the metallic iron and the acid and hydrogen gas is generated. Since the chemical potential of hydrogen in the pickling solution is higher than that of hydrogen in the steel to be pickled, the generated hydrogen permeates into the steel and accumulates to cause hydrogen embrittlement, thereby affecting the mechanical properties of the steel or the subsequent processing.
The method comprises the steps of mixing water, a silane coupling agent, water-soluble silicate, an accelerator, a silicon oxide filler and water-soluble film-forming resin uniformly in sequence; the water-soluble film-forming resin contains water-soluble polyurethane resin, but cannot achieve better corrosion resistance and has poorer adhesive force. Therefore, it is necessary to develop a water-based antirust sealing agent with good adhesion and corrosion resistance.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of poor adhesive force effect and poor corrosion resistance of the existing commonly used water-based antirust sealing agent, the water-based antirust sealing agent is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
an aqueous antirust sealing agent comprises the following components: 3~6 parts of oleic acid, 4~8 parts of diisopropanolamine, 1~4 parts of hexamethylenetetramine, 20~30 parts of water, its characterized in that still includes: 20-35 parts of a composite antirust component A and 15-30 parts of a composite antirust component B.
The preparation method of the composite antirust component A comprises the following steps:
(1) at the temperature of 30-45 ℃, according to the mass ratio of 7: 3: 0.01-0.04 mixing and stirring polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, carrying out temperature programming, keeping the temperature to obtain a prepolymer, mixing and stirring dimethylformamide accounting for 30-45% of the mass of the prepolymer, carrying out volatilization reaction, and carrying out heat treatment to obtain polyurethane urea;
(2) according to the mass ratio of 1: 8-12 mixing and stirring sodium alginate and water, standing for swelling, adding periodic acid with the mass being 10-15% of that of the sodium alginate, heating, stirring, adding microcrystalline cellulose with the mass being 40-60% of that of the sodium alginate, stirring for reaction, discharging, and obtaining sodium alginate dispersion liquid, wherein the mass ratio of the sodium alginate to the water is 7: 2-4: 1 mixing the sodium alginate dispersion liquid, the polyurethane urea and the reagent A, evaporating under reduced pressure, and collecting the concentrated solution, namely the composite antirust component A.
The chain extender in the step (1): ventilating and protecting at the temperature of 30-45 ℃, wherein the mass ratio of (5): and 1-3, mixing and stirring isophorone diisocyanate and acrylonitrile, reacting at room temperature, heating to react, and vacuumizing and drying to obtain the chain extender.
The reagent A in the step (2): according to the mass ratio of 1: 8-12, mixing dopamine hydrochloride and water to obtain a dopamine solution, and mixing the dopamine solution according to a volume ratio of 10: 1: and (3) mixing absolute ethyl alcohol and ammonia water to obtain a reagent A.
The preparation of the composite antirust component B comprises the following steps: at the temperature of 30-45 ℃, according to the mass ratio of 1: 5-8, mixing water glass and water, heating, adding benzotriazole accounting for 6-10% of the mass of the water glass and boric acid accounting for 2-5% of the mass of the water glass, mixing and stirring to obtain a base material, and taking the base material according to the mass ratio of 10-15: 1: 0.1-0.3, adding EDTA and an auxiliary agent, mixing to obtain a mixture, adding a prefabricated surfactant accounting for 20-30% of the mass of the mixture, a reagent B accounting for 2-5% of the mass of the mixture and aluminum powder slurry accounting for 10-15% of the mass of the mixture into the mixture, mixing, shearing and dispersing to obtain a dispersion, and performing microwave treatment on the dispersion to obtain the composite antirust component B.
The auxiliary agent is as follows: according to the mass ratio of 3: 1-2: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
The reagent B: according to the mass ratio of 1: 1-3: 8: and 20-30, mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B.
And the aluminum powder slurry: according to the mass parts, 10-20 parts of aluminum powder, 3-6 parts of titanate coupling agent, 8-12 parts of glycerol and 40-60 parts of ethanol solution are mixed, and the mixture is subjected to heat preservation treatment at 30-45 ℃, ultrasonic dispersion and discharging to obtain aluminum powder slurry.
The pre-formed surfactant: according to the mass ratio of 1: 2-4: 0.01 mixing oleic acid, N-dimethyl-1, 3-propane diamine and NaF, stirring and reacting at 155-165 ℃ under the protection of argon, distilling under reduced pressure to obtain a crude product, performing neutral alumina column chromatography on the crude product, leaching with a mixed washing solution 4-8 times the mass of the crude product, and collecting a column-passing solution to obtain the prefabricated surfactant.
The volume ratio of the components is 3: and 1-2, mixing methanol and dichloromethane to obtain a mixed washing liquid.
Compared with other methods, the method has the beneficial technical effects that:
(1) in the invention, sodium alginate is dispersed by ultrasonic waves, the o-diol structure of the sodium alginate is changed into a dialdehyde group structure under the oxidation of sodium periodate, so that the sodium alginate is changed into polyaldehyde sodium alginate, aldehyde groups in the polyaldehyde sodium alginate can be partially subjected to aldol condensation with active hydroxyl groups in microcrystalline cellulose in the subsequent reaction process, and chemical bonding is formed between the polyaldehyde sodium alginate and the microcrystalline cellulose, thereby improving the mechanical property of the polyaldehyde sodium alginate on the surface of steel during use, and meanwhile, if a small amount of ferric oxide components appear on the surface of the steel in the subsequent use process, acid components in the system can enable the Fe component to be Fe in the system3+Dissolving out, further generating chemical bonding with a polyaldehyde sodium alginate structure, enhancing the bonding force among alginate chains through chelation, greatly improving the stability of the closed antirust film, further enhancing the adhesive force of the closed antirust film, and effectively reducing the possibility of corrosion by the adsorption and fixation of free iron ions;
(2) the aluminum powder slurry is prepared by taking aluminum powder as a raw material, after the aluminum powder is treated by glycerol and a titanate coupling agent, the surface of the aluminum powder can be protected from being corroded in the processing and using processes, the adhesive force of the aluminum powder and the polyurethane urea in the composite antirust component A is improved, under the action of the titanate coupling agent, a bridge is formed between the polyurethane urea and the aluminum powder, and the dopamine hydrochloride in a matching agent A is self-oxidized into poly-dopamine, so that the whole antirust film layer is more complete and continuous, the aluminum powder is tightly and uniformly arranged in the polyurethane powder, the anticorrosion effect of the closed antirust film can be improved, a corrosion medium can permeate from the outer surface to the inner surface only by bypassing the aluminum powder layer, the impermeability of the antirust film is greatly improved, and the adhesion, corrosion resistance and other properties after the antirust film is used are.
Detailed Description
Mixing washing liquor: according to the volume ratio of 3: and 1-2, mixing methanol and dichloromethane to obtain a mixed washing liquid.
Chain extender: introducing argon at the temperature of 30-45 ℃ under the protection of argon, and mixing the following components in a mass ratio of 5: 1-3, mixing isophorone diisocyanate and acrylonitrile, magnetically stirring for 20-35 min at the speed of 300-500 r/min, reacting for 20-24 h at room temperature, reacting for 12-15 h at the temperature of 40-50 ℃, and then vacuumizing and drying at the temperature of 60-70 ℃ to constant weight to obtain the chain extender.
Reagent A: according to the mass ratio of 1: 8-12, mixing dopamine hydrochloride and deionized water to obtain a dopamine solution, and mixing the dopamine solution according to a volume ratio of 10: 1: and (3) mixing absolute ethyl alcohol and ammonia water with the concentration of 0.1mol/L to obtain a reagent A.
And (3) reagent B: according to the mass ratio of 1: 1-3: 8: and 20-30, mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3: 1-2: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
Pre-surfactant preparation: according to the mass ratio of 1: 2-4: 0.01 taking oleic acid, N-dimethyl-1, 3-propane diamine and NaF to mix in a container, stirring and reacting for 8-12 h at the temperature of 300-500 r/min under the protection of argon at the temperature of 155-165 ℃, distilling at the temperature of 55-70 ℃ under reduced pressure until the weight is constant to obtain a crude product, taking the crude product to perform chromatography on a neutral alumina column, leaching with a mixed washing solution 4-8 times the mass of the crude product, and collecting a column-passing solution to obtain the prefabricated surfactant.
Aluminum powder slurry: according to the mass parts, 10-20 parts of aluminum powder with the particle size of 0.02-0.06 mm, 3-6 parts of titanate coupling agent, 8-12 parts of glycerol and 40-60 parts of ethanol solution with the volume fraction of 60% are mixed in a reaction kettle, heat preservation treatment is carried out for 20-45 min at the temperature of 30-45 ℃, then the mixture is moved into an ultrasonic dispersion instrument, ultrasonic dispersion is carried out for 15-35 min under the frequency condition of 45-55 kHz, and discharging is carried out, so that aluminum powder slurry is obtained.
The preparation method of the composite antirust component A comprises the following steps:
(1) and (2) in a water bath at the temperature of 30-45 ℃, according to the mass ratio of 7: 3: 0.01-0.04, mixing and stirring polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, heating to 80-90 ℃ at a temperature of 4-8 ℃/min, keeping the temperature for 15-30 min to obtain a prepolymer, uniformly mixing and stirring dimethylformamide accounting for 30-45% of the mass of the prepolymer, pouring the mixture into a polytetrafluoroethylene grinding tool, volatilizing at 50-60 ℃ for 24-36 h, treating at a vacuum degree of 0.1MPa and a vacuum degree of 80-100 ℃ for 1-3 h, and carrying out heat treatment to constant weight to obtain polyurethane urea;
(2) according to the mass ratio of 1: 8-12 mixing sodium alginate and water in a container, stirring for 20-45 min at a speed of 300-500 r/min, standing for swelling for 3-5 h, adding periodic acid with the mass being 10-15% of that of the sodium alginate, heating to 75-85 ℃, heating to 400-600 r/min, stirring for reaction for 2-4, adding microcrystalline cellulose with the mass being 40-60% of that of the sodium alginate, stirring for reaction for 3-5 h, discharging, and obtaining a sodium alginate dispersion solution, wherein the mass ratio of the sodium alginate dispersion solution to the water is 7: 2-4: 1, mixing the sodium alginate dispersion liquid, the polyurethane urea and the reagent A, vacuumizing at 40-60 ℃, decompressing and evaporating to 30-45% of the original volume, and collecting a concentrated solution, namely the composite antirust component A.
Preparing a composite antirust component B: and (2) in a water bath at the temperature of 30-45 ℃, according to the mass ratio of 1: 5-8, mixing water glass and deionized water, heating to 55-70 ℃, adding benzotriazole accounting for 6-10% of the mass of the water glass and boric acid accounting for 2-5% of the mass of the water glass, mixing, stirring for 30-55 min at 300-500 r/min to obtain a base material, and taking the base material according to the mass ratio of 10-15: 1: 0.1-0.3, adding EDTA and an auxiliary agent, mixing to obtain a mixture, adding a prefabricated surfactant accounting for 20-30% of the mass of the mixture, a reagent B accounting for 2-5% of the mass of the mixture and aluminum powder slurry accounting for 10-15% of the mass of the mixture into the mixture, mixing, shearing and dispersing for 5-10 min at 2000-3000 r/min to obtain a dispersion, and treating the dispersion for 6-10 min by using 300W microwaves to obtain a composite antirust component B.
The water-based antirust sealing agent comprises the following components in parts by weight: 3-6 parts of oleic acid, 4-8 parts of diisopropanolamine, 1-4 parts of hexamethylenetetramine, 20-30 parts of water, 20-35 parts of a composite antirust component A and 15-30 parts of a composite antirust component B.
A preparation method of a water-based antirust sealing agent comprises the following steps:
(1) taking 3-6 parts of oleic acid, 4-8 parts of diisopropanolamine, 1-4 parts of hexamethylenetetramine, 20-30 parts of water, 20-35 parts of a composite antirust component A and 15-30 parts of a composite antirust component B in parts by mass;
(2) mixing oleic acid, diisopropanolamine, water and the composite antirust component A in a reaction kettle at the temperature of 30-45 ℃ in a water bath, magnetically stirring for 25-50 min at the speed of 300-500 r/min, heating to 55-70 ℃, adding the composite antirust component B and hexamethylenetetramine, mixing, and carrying out ultrasonic treatment at the frequency of 45-55 kHz for 15-25 min to obtain the water-based antirust sealing agent.
Mixing washing liquor: according to the volume ratio of 3: 1, mixing methanol and dichloromethane to obtain a mixed washing liquid.
Chain extender: introducing argon at 30 ℃ under the protection of argon, and mixing the components in a mass ratio of 5: 1 mixing isophorone diisocyanate and acrylonitrile, magnetically stirring for 20min at 300r/min, reacting for 20h at room temperature, reacting for 12h at 40 ℃, and then vacuumizing and drying at 60 ℃ to constant weight to obtain the chain extender.
Reagent A: according to the mass ratio of 1: 8, mixing dopamine hydrochloride and deionized water to obtain dopamine solution, wherein the dopamine solution is prepared from the following raw materials in a volume ratio of 10: 1: 1, mixing absolute ethyl alcohol and ammonia water with the concentration of 0.1mol/L to obtain a reagent A.
And (3) reagent B: according to the mass ratio of 1: 1: 8: 20 mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3: 1: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
Pre-surfactant preparation: according to the mass ratio of 1: 2: 0.01 taking oleic acid, N-dimethyl-1, 3-propane diamine and NaF to mix in a container, stirring and reacting for 8 hours at the temperature of 300r/min under the protection of argon at the temperature of 155 ℃, distilling at the temperature of 55 ℃ under reduced pressure until the weight is constant to obtain a crude product, taking the crude product to perform chromatography on a neutral alumina column, leaching with mixed washing liquor with the mass of 4 times of that of the crude product, and collecting column-passing liquor to obtain the prefabricated surfactant.
Aluminum powder slurry: according to the mass parts, 10 parts of aluminum powder with the particle size of 0.02mm, 3 parts of titanate coupling agent, 8 parts of glycerol and 40 parts of ethanol solution with the volume fraction of 60% are mixed in a reaction kettle, the mixture is subjected to heat preservation treatment at 30 ℃ for 20min, then the mixture is transferred into an ultrasonic dispersion instrument, ultrasonic dispersion is carried out for 15min under the condition of 45kHz frequency, and discharging is carried out, so that the aluminum powder slurry is obtained.
The preparation method of the composite antirust component A comprises the following steps:
(1) performing water bath at 30 ℃, and mixing the raw materials in a mass ratio of 7: 3: 0.01 taking polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, mixing and stirring, heating to 80 ℃ by a program of 4 ℃/min, keeping the temperature for 15min to obtain a prepolymer, taking dimethylformamide accounting for 30% of the mass of the prepolymer, mixing and stirring uniformly, pouring into a polytetrafluoroethylene grinding tool, volatilizing at 50 ℃ for 24h, treating at 80 ℃ and a vacuum degree of 0.1MPa for 1h to obtain polyurethane urea;
(2) according to the mass ratio of 1: mixing sodium alginate and water in a container, stirring for 20min at a speed of 300r/min, standing and swelling for 3h, adding periodic acid with the mass of 10% of the sodium alginate, heating to 75 ℃, heating and stirring for reaction for 2h at a speed of 400r/min, adding microcrystalline cellulose with the mass of 40% of the sodium alginate, stirring for reaction for 3h, discharging to obtain a sodium alginate dispersion liquid, and mixing the sodium alginate dispersion liquid and the water in a mass ratio of 7: 2: 1 mixing the sodium alginate dispersion liquid, the polyurethane urea and the reagent A, vacuumizing at 40 ℃, decompressing and evaporating to 30% of the original volume, and collecting the concentrated solution, namely the composite antirust component A.
Preparing a composite antirust component B: performing water bath at 30 ℃, and mixing the raw materials in a mass ratio of 1: 5, mixing water glass and deionized water, heating to 55 ℃, adding benzotriazole accounting for 6 percent of the mass of the water glass and boric acid accounting for 2 percent of the mass of the water glass, mixing, stirring at 300r/min for 30min to obtain a base material, and taking the base material according to the mass ratio of 10: 1: 0.1, adding EDTA and an auxiliary agent, mixing to obtain a mixture, taking the mixture, adding a prefabricated surfactant accounting for 20% of the mass of the mixture, a reagent B accounting for 2% of the mass of the mixture and aluminum powder slurry accounting for 10% of the mass of the mixture, mixing, shearing and dispersing at 2000r/min for 5min to obtain a dispersion, taking the dispersion, and performing microwave treatment at 300W for 6min to obtain the composite antirust component B.
The water-based antirust sealing agent comprises the following components in parts by weight: 3 parts of oleic acid, 4 parts of diisopropanolamine, 1 part of hexamethylenetetramine, 20 parts of water, 20 parts of a composite antirust component A and 15 parts of a composite antirust component B.
A preparation method of a water-based antirust sealing agent comprises the following steps:
(1) taking 3 parts of oleic acid, 4 parts of diisopropanolamine, 1 part of hexamethylenetetramine, 20 parts of water, 20 parts of composite antirust component A and 15 parts of composite antirust component B in parts by mass;
(2) and mixing oleic acid, diisopropanolamine, water and the composite antirust component A in a reaction kettle at the temperature of 30 ℃ in a water bath, magnetically stirring for 25min at the speed of 300r/min, heating to 55 ℃, adding the composite antirust component B and hexamethylenetetramine, mixing, and carrying out ultrasonic treatment for 15min at the frequency of 45kHz to obtain the water-based antirust sealing agent.
Mixing washing liquor: according to the volume ratio of 3: 1.5 mixing methanol and dichloromethane to obtain mixed washing liquid.
Chain extender: introducing argon at 38 ℃ under the protection of argon, and mixing the components in a mass ratio of 5: 2 mixing isophorone diisocyanate and acrylonitrile, magnetically stirring for 30min at 400r/min, reacting for 22h at room temperature, reacting for 13h at 45 ℃, and then vacuumizing and drying at 65 ℃ to constant weight to obtain the chain extender.
Reagent A: according to the mass ratio of 1: 10, mixing dopamine hydrochloride and deionized water to obtain dopamine solution, wherein the dopamine solution is prepared from the following components in a volume ratio of 10: 1: 2, mixing absolute ethyl alcohol and ammonia water with the concentration of 0.1mol/L to obtain the reagent A.
And (3) reagent B: according to the mass ratio of 1: 2: 8: 25 mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3: 1.5: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
Pre-surfactant preparation: according to the mass ratio of 1: 3: 0.01 taking oleic acid, N-dimethyl-1, 3-propane diamine and NaF to mix in a container, stirring and reacting for 10 hours at 160 ℃ at a speed of 400r/min under the protection of argon, carrying out reduced pressure distillation at 60 ℃ to constant weight to obtain a crude product, taking the crude product to carry out chromatography on a neutral alumina column, carrying out leaching by using a mixed washing solution with the mass of 6 times of the crude product, and collecting a column passing solution to obtain the prefabricated surfactant.
Aluminum powder slurry: taking 15 parts of aluminum powder with the particle size of 0.04mm, 5 parts of titanate coupling agent, 10 parts of glycerol and 50 parts of ethanol solution with the volume fraction of 60% to mix in a reaction kettle, carrying out heat preservation treatment at 38 ℃ for 30min, transferring into an ultrasonic dispersion instrument, carrying out ultrasonic dispersion for 25min under the condition of 50kHz frequency, and discharging to obtain aluminum powder slurry.
The preparation method of the composite antirust component A comprises the following steps:
(1) performing water bath at 40 ℃, and mixing the raw materials in a mass ratio of 7: 3: 0.03 taking polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, mixing and stirring, heating to 85 ℃ by a program of 6 ℃/min, preserving heat for 20min to obtain a prepolymer, taking dimethylformamide accounting for 40% of the mass of the prepolymer, mixing and stirring uniformly, pouring into a polytetrafluoroethylene grinding tool, volatilizing at 55 ℃ for reaction for 32h, treating at 90 ℃ and a vacuum degree of 0.1MPa for 2h, and carrying out heat treatment to constant weight to obtain polyurethane urea;
(2) according to the mass ratio of 1: mixing sodium alginate and water in a container, stirring for 40min at a speed of 400r/min, standing and swelling for 4h, adding periodic acid accounting for 13% of the mass of the sodium alginate, heating to 80 ℃, heating and stirring for reaction for 3h at a speed of 500r/min, adding microcrystalline cellulose accounting for 50% of the mass of the sodium alginate, stirring for reaction for 4h, discharging to obtain a sodium alginate dispersion, and mixing the sodium alginate dispersion with the water in a mass ratio of 7: 3: 1 mixing the sodium alginate dispersion liquid, the polyurethane urea and the reagent A, vacuumizing at 50 ℃, decompressing and evaporating to 35 percent of the original volume, and collecting the concentrated solution, namely the composite antirust component A.
Preparing a composite antirust component B: heating in water bath at 38 ℃, and mixing the raw materials in a mass ratio of 1: 6, mixing water glass and deionized water, heating to 60 ℃, adding benzotriazole accounting for 8% of the mass of the water glass and boric acid accounting for 4% of the mass of the water glass, mixing, stirring at 400r/min for 40min to obtain a base material, and taking the base material according to the mass ratio of 13: 1: 0.2, adding EDTA and an auxiliary agent, mixing to obtain a mixture, adding a prefabricated surfactant accounting for 25% of the mass of the mixture, a reagent B accounting for 4% of the mass of the mixture and aluminum powder slurry accounting for 13% of the mass of the mixture into the mixture, mixing, shearing and dispersing at 2500r/min for 8min to obtain a dispersion liquid, and treating the dispersion liquid with 300W microwaves for 8min to obtain the composite antirust component B.
The water-based antirust sealing agent comprises the following components in parts by weight: 5 parts of oleic acid, 6 parts of diisopropanolamine, 3 parts of hexamethylenetetramine, 25 parts of water, 30 parts of a composite antirust component A and 25 parts of a composite antirust component B.
A preparation method of a water-based antirust sealing agent comprises the following steps:
(1) taking 5 parts of oleic acid, 6 parts of diisopropanolamine, 3 parts of hexamethylenetetramine, 25 parts of water, 29 parts of a composite antirust component A and 25 parts of a composite antirust component B in parts by weight;
(2) mixing oleic acid, diisopropanolamine, water and the composite antirust component A in a reaction kettle at 35 ℃ in a water bath, magnetically stirring for 35min at 400r/min, heating to 65 ℃, adding the composite antirust component B and hexamethylenetetramine, mixing, and performing ultrasonic treatment at 50kHz frequency for 20min to obtain the water-based antirust sealing agent.
Mixing washing liquor: according to the volume ratio of 3: and 2, mixing methanol and dichloromethane to obtain a mixed washing liquid.
Chain extender: introducing argon at 45 ℃ under the protection of argon, and mixing the components in a mass ratio of 5: 3 mixing isophorone diisocyanate and acrylonitrile, magnetically stirring for 35min at 500r/min, reacting for 24h at room temperature, reacting for 15h at 50 ℃, and then vacuumizing and drying at 70 ℃ to constant weight to obtain the chain extender.
Reagent A: according to the mass ratio of 1: 12, mixing dopamine hydrochloride and deionized water to obtain dopamine solution, wherein the dopamine solution is prepared from the following raw materials in a volume ratio of 10: 1: 3, mixing absolute ethyl alcohol and ammonia water with the concentration of 0.1mol/L to obtain the reagent A.
And (3) reagent B: according to the mass ratio of 1: 3: 8: 30 mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3: 2: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
Pre-surfactant preparation: according to the mass ratio of 1: 4: 0.01 taking oleic acid, N-dimethyl-1, 3-propane diamine and NaF to mix in a container, stirring and reacting for 12h at 165 ℃ at 500r/min under the protection of argon, carrying out reduced pressure distillation at 70 ℃ to constant weight to obtain a crude product, taking the crude product to carry out chromatography on a neutral alumina column, carrying out leaching by using mixed washing liquor with the mass of 8 times of that of the crude product, and collecting column-passing liquor to obtain the prefabricated surfactant.
Aluminum powder slurry: according to the mass parts, 20 parts of aluminum powder with the particle size of 0.06mm, 6 parts of titanate coupling agent, 12 parts of glycerol and 60 parts of ethanol solution with the volume fraction of 60% are mixed in a reaction kettle, the mixture is subjected to heat preservation treatment at 45 ℃ for 45min, then the mixture is transferred into an ultrasonic dispersion instrument, ultrasonic dispersion is carried out for 35min under the frequency condition of 55kHz, and the aluminum powder slurry is obtained after discharging.
The preparation method of the composite antirust component A comprises the following steps:
(1) performing mixing in a water bath at 45 ℃ according to a mass ratio of 7: 3: 0.04 mixing and stirring polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, heating to 90 ℃ at the program of 8 ℃/min, keeping the temperature for 30min to obtain a prepolymer, uniformly mixing and stirring dimethylformamide accounting for 45% of the mass of the prepolymer, pouring the mixture into a polytetrafluoroethylene grinding tool, volatilizing and reacting for 36h at the temperature of 60 ℃, treating for 3h at the vacuum degree of 0.1MPa and the temperature of 100 ℃ to reach constant weight, and obtaining polyurethane urea;
(2) according to the mass ratio of 1: 12 mixing sodium alginate and water in a container, stirring for 45min at a speed of 500r/min, standing and swelling for 5h, adding periodic acid accounting for 15% of the mass of the sodium alginate, heating to 85 ℃, heating and stirring for reaction for 4h at a speed of 600r/min, adding microcrystalline cellulose accounting for 60% of the mass of the sodium alginate, stirring for reaction for 5h, discharging to obtain a sodium alginate dispersion liquid, and mixing the sodium alginate dispersion liquid and the water in a mass ratio of 7: 4: 1 mixing the sodium alginate dispersion liquid, the polyurethane urea and the reagent A, vacuumizing at 60 ℃, decompressing and evaporating to 45 percent of the original volume, and collecting the concentrated solution to obtain the composite antirust component A.
Preparing a composite antirust component B: performing mixing in a water bath at 45 ℃ according to a mass ratio of 1: 8, mixing water glass and deionized water, heating to 70 ℃, adding benzotriazole accounting for 10 percent of the mass of the water glass and boric acid accounting for 5 percent of the mass of the water glass, mixing, stirring at 500r/min for 55min to obtain a base material, and taking the base material according to the mass ratio of 15: 1: 0.3, adding EDTA and an auxiliary agent, mixing to obtain a mixture, taking the mixture, adding a prefabricated surfactant accounting for 30% of the mass of the mixture, a reagent B accounting for 5% of the mass of the mixture and aluminum powder slurry accounting for 15% of the mass of the mixture, mixing, shearing and dispersing at 3000r/min for 10min to obtain a dispersion liquid, taking the dispersion liquid, and performing microwave treatment at 300W for 10min to obtain the composite antirust component B.
The water-based antirust sealing agent comprises the following components in parts by weight: 6 parts of oleic acid, 8 parts of diisopropanolamine, 4 parts of hexamethylenetetramine, 30 parts of water, 35 parts of a composite antirust component A and 30 parts of a composite antirust component B.
A preparation method of a water-based antirust sealing agent comprises the following steps:
(1) taking 6 parts of oleic acid, 8 parts of diisopropanolamine, 4 parts of hexamethylenetetramine, 30 parts of water, 35 parts of a composite antirust component A and 30 parts of a composite antirust component B in parts by mass;
(2) at the temperature of 45 ℃ in water bath, firstly, mixing oleic acid, diisopropanolamine, water and the composite antirust component A in a reaction kettle, magnetically stirring for 50min at the speed of 500r/min, heating to 70 ℃, adding the composite antirust component B and hexamethylenetetramine, mixing, and carrying out ultrasonic treatment at the frequency of 55kHz for 25min to obtain the water-based antirust sealing agent.
Comparative example 1: basically the same procedure as in example 1 was conducted except that the composite rust inhibitive component A was not present.
Comparative example 2: basically the same procedure as in example 1 was conducted except that the composite rust inhibitive component B was absent.
Comparative example 3: antirust sealing agent produced by a certain company in the Wuxi market.
The water-based antirust sealing agent obtained in the examples and the water-based antirust sealing agent obtained in the comparative example are subjected to a neutral salt spray test according to the requirements specified in GB/T101251997, and the water-based antirust sealing agent is qualified according to the salt spray test of 120h, wherein the corrosion area is less than 3%. The test results are shown in table 1.
Table 1:
| test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Adhesion (grade) | 0 | 0 | 0 | 0 | 0 | 2 |
| Percent of pass (%) of corrosion resistance (120 days) | 100 | 97 | 99 | 95 | 94 | 69 |
| Whether benzene and other harmful solvents are contained | Does not contain | Does not contain | Does not contain | Does not contain | Does not contain | Comprises |
In sum, compared with the commercially available product, the aqueous antirust sealing agent disclosed by the invention has a better effect and is worthy of great popularization.
Claims (5)
1. The water-based antirust sealing agent comprises the following components in parts by weight: 3~6 parts of oleic acid, 4~8 parts of diisopropanolamine, 1~4 parts of hexamethylenetetramine, 20~30 parts of water, its characterized in that still includes: 20-35 parts of a composite antirust component A and 15-30 parts of a composite antirust component B;
the preparation of the composite antirust component B comprises the following steps: at the temperature of 30-45 ℃, according to the mass ratio of 1: 5-8, mixing water glass and water, heating, adding benzotriazole accounting for 6-10% of the mass of the water glass and boric acid accounting for 2-5% of the mass of the water glass, mixing and stirring to obtain a base material, and taking the base material according to the mass ratio of 10-15: 1: 0.1-0.3, adding EDTA and an auxiliary agent, mixing to obtain a mixture, adding a prefabricated surfactant accounting for 20-30% of the mass of the mixture, a reagent B accounting for 2-5% of the mass of the mixture and aluminum powder slurry accounting for 10-15% of the mass of the mixture into the mixture, mixing, shearing and dispersing to obtain a dispersion, and performing microwave treatment on the dispersion to obtain a composite antirust component B; the reagent B: according to the mass ratio of 1: 1-3: 8: 20-30, mixing sodium molybdate, sodium benzoate, sodium carbonate and water to obtain a reagent B; the aluminum powder slurry: mixing 10-20 parts of aluminum powder, 3-6 parts of titanate coupling agent, 8-12 parts of glycerol and 40-60 parts of ethanol solution by weight, carrying out heat preservation treatment at 30-45 ℃, carrying out ultrasonic dispersion, and discharging to obtain aluminum powder slurry;
the preparation method of the composite antirust component A comprises the following steps:
(1) at the temperature of 30-45 ℃, according to the mass ratio of 7: 3: 0.01-0.04 mixing and stirring polyoxypropylene glycol, a chain extender and dibutyl tin dilaurate, carrying out temperature programming, keeping the temperature to obtain a prepolymer, mixing and stirring dimethylformamide accounting for 30-45% of the mass of the prepolymer, carrying out volatilization reaction, and carrying out heat treatment to obtain polyurethane urea;
(2) according to the mass ratio of 1: 8-12 mixing and stirring sodium alginate and water, standing for swelling, adding periodic acid with the mass being 10-15% of that of the sodium alginate, heating, stirring, adding microcrystalline cellulose with the mass being 40-60% of that of the sodium alginate, stirring for reaction, discharging, and obtaining sodium alginate dispersion liquid, wherein the mass ratio of the sodium alginate to the water is 7: 2-4: 1, mixing sodium alginate dispersion liquid, polyurethane urea and a reagent A, evaporating under reduced pressure, and collecting a concentrated solution, namely a composite antirust component A; the reagent A is: according to the mass ratio of 1: 8-12, mixing dopamine hydrochloride and water to obtain a dopamine solution, and mixing the dopamine solution according to a volume ratio of 10: 1: and (3) mixing absolute ethyl alcohol and ammonia water to obtain a reagent A.
2. The aqueous rust inhibitive sealant according to claim 1, wherein the chain extender in step (1): ventilating and protecting at the temperature of 30-45 ℃, wherein the mass ratio of (5): and 1-3, mixing and stirring isophorone diisocyanate and acrylonitrile, reacting at room temperature, heating to react, and vacuumizing and drying to obtain the chain extender.
3. The aqueous rust inhibitive sealant according to claim 1, wherein the auxiliary agent: according to the mass ratio of 3: 1-2: 1 taking ZnCl2Sodium citrate, NH4And mixing Cl to obtain the auxiliary agent.
4. The aqueous rust inhibitive sealant according to claim 1, wherein the pre-surfactant: according to the mass ratio of 1: 2-4: 0.01 mixing oleic acid, N-dimethyl-1, 3-propane diamine and NaF, stirring and reacting at 155-165 ℃ under the protection of argon, distilling under reduced pressure to obtain a crude product, performing neutral alumina column chromatography on the crude product, leaching with a mixed washing solution 4-8 times the mass of the crude product, and collecting a column-passing solution to obtain the prefabricated surfactant.
5. The aqueous antirust sealing agent according to claim 4, wherein the mixed lotion is prepared by mixing the following components in a volume ratio of 3: and 1-2, mixing methanol and dichloromethane to obtain a mixed washing liquid.
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