CN114231096A - Fireproof powder coating and preparation method thereof - Google Patents

Fireproof powder coating and preparation method thereof Download PDF

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Publication number
CN114231096A
CN114231096A CN202111541311.5A CN202111541311A CN114231096A CN 114231096 A CN114231096 A CN 114231096A CN 202111541311 A CN202111541311 A CN 202111541311A CN 114231096 A CN114231096 A CN 114231096A
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parts
divalent metal
liquid
powder coating
polyion liquid
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刘建良
邹小敏
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JIANGXI RUIKESI TECHNOLOGY CO LTD
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JIANGXI RUIKESI TECHNOLOGY CO LTD
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    • C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
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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 relates to the technical field of coatings, and provides a fireproof powder coating which comprises the following raw materials in parts by weight: 40-80 parts of divalent metal/polyion liquid-alkenyl resin particles, 2-8 parts of polyion liquid, 8-20 parts of cross-linking agent and hydrophobic SiO2‑TiO28-15 parts of composite gel, 8-15 parts of ammonium dihydrogen phosphate, 3-10 parts of magnesium oxide, 3-10 parts of montmorillonite, 2-8 parts of barium sulfate whisker, 1-5 parts of silicon nitride, 2-8 parts of curing agent and 3-10 parts of auxiliary agent. The coating film obtained by the coating disclosed by the invention has excellent corrosion resistance, high surface resistance and high toughness, and can adapt to various service environments.

Description

Fireproof powder coating and preparation method thereof
Technical Field
The invention relates to the technical field of coatings, in particular to a fireproof powder coating and a preparation method thereof.
Background
At present, thermosetting powder coating is the most advanced and environment-friendly coating in domestic and foreign coatings, mainly because the coating is complete solid powder, does not contain any volatile solution and moisture, and is far more excellent in the performance of various physical and chemical properties than other coatings. Due to the thermosetting property of the powder coating, after heating and baking, three-dimensional net-shaped crosslinking is carried out, and an excellent and complete coating film is formed.
The powder coating capable of eliminating static electricity is a powder coating which has certain current conduction and charge dissipation functions after being sprayed on a substrate to form a film, can be used for eliminating static electricity, electromagnetic shielding, electric heating and corrosion prevention, and has wide application in the fields of buildings, transportation, military, modern electronics and the like. However, the film forming substances of the existing powder coating are various and the conductive filler has defects, so that the antistatic performance of the powder coating is poor; moreover, the corrosion resistance is not ideal, resulting in a reduced service life.
Disclosure of Invention
The present invention is directed to overcome at least one of the above disadvantages and drawbacks of the prior art, and to provide a fireproof powder coating and a method for preparing the same. The purpose of the invention is realized based on the following technical scheme:
in one aspect, the invention provides a fireproof powder coating, which comprises the following raw materials in parts by weight: 40-80 parts of divalent metal/polyion liquid-alkenyl resin particles, 2-8 parts of polyion liquid, 8-20 parts of cross-linking agent and hydrophobic SiO2-TiO28-15 parts of composite gel, 8-15 parts of ammonium dihydrogen phosphate, 3-10 parts of magnesium oxide, 3-10 parts of montmorillonite, 2-8 parts of barium sulfate whisker, 1-5 parts of silicon nitride, 2-8 parts of a curing agent and 3-10 parts of an auxiliary agent, wherein the auxiliary agent comprises one or more of a dispersing agent, a leveling agent, a defoaming agent and a flame retardant.
According to the invention, divalent metal is added into the resin coating, so that the electrical property and the mechanical property of the coating can be effectively improved, and the divalent metal/polyion liquid-alkenyl resin particles are adopted to coat the polyion liquid and the alkenyl resin on the surface of the divalent metal, so that the problems of uneven distribution of metal particles in the resin material, and poor macromolecule aggregation and modification effect are solved. The polyion liquid has excellent mechanical stability, ionic conductivity, processability, durability, chemical compatibility, controllability and the like, and can optimize and improve the performance of resin materials. According to the invention, a part of polyion liquid is used for coating the divalent metal, a staggered complex structure is formed with the resin material, the divalent metal is coated and modified together, the structure of the resin material is improved and repaired, and the structural strength of the resin material is improved. Part of polyion liquid is used as a raw material of the coating and is crosslinked with divalent metal/polyion liquid-alkenyl resin particles and the like; the polyionic liquid has excellent performances of both the ionic liquid and the polymer, not only promotes the curing of the epoxy resin, but also can be used as a toughening agent to be compounded with the alkenyl resin, the composite gel and the like, so that the crosslinking density and the glass transition temperature of the alkenyl resin are effectively improved, and the flexibility of the alkenyl resin is improved.
Hydrophobic SiO2-TiO2SiO in composite gels2And TiO2Inorganic particles can improve the antistatic property and the wear resistance of the coating; TiO 22Has the advantages ofDifferent photocatalytic ability, can photocatalytically decompose some organic matters of bacteria, thereby achieving the antibacterial effect, TiO2The coating can also be used as an anti-ultraviolet agent to improve the weather resistance of the coating and as a pigment to endow the coating with color; SiO 22The gel contains two positively charged N+Ions can selectively adsorb with negatively charged cell walls on the cell surface, penetrate through the surface to enter cell membranes through the functions of permeation and diffusion, so as to block the semi-permeation function of the cell membranes, further penetrate into the cells, passivate cellular enzymes, and cannot generate the protease, so that the protein is denatured to kill bacterial cells; added in the form of composite gel, improves SiO2And TiO2The compatibility of the inorganic particles and the alkenyl resin endows the coating with excellent corrosion resistance, effectively improves the flexibility of the obtained coating, and can adapt to various service environments; after the composite gel is subjected to hydrophobic treatment, the adhesive force, the moisture resistance and the stain resistance of the obtained coating film can be improved. The ammonium dihydrogen phosphate has fireproof performance, can be used as a dispersant of the coating, and can also improve the corrosion resistance of the coating. The magnesium oxide has high fireproof and insulating properties, can improve the compactness and rheological property of a coating, and can improve the wear resistance of the coating under the combined action of the magnesium oxide and silicon nitride. The montmorillonite can improve the antistatic property of the coating, and the barium sulfate whisker not only has excellent weather resistance and ageing resistance, but also can increase the wear resistance and impact strength of the coating, obviously improve the toughness of the coating and obviously improve the surface smoothness. The invention greatly improves the comprehensive performance of the coating by compounding various raw materials.
Preferably, the divalent metal comprises one or more of titanium oxide, copper oxide, iron oxide, zinc oxide, magnesium oxide, calcium carbonate, barium sulfate.
Preferably, the monomer of the alkenyl resin includes one or more of styrene, butyl methacrylate, butyl acrylate, methyl methacrylate and methyl acrylate, and one or more of hydroxyethyl methacrylate and hydroxyethyl acrylate.
Preferably, the content of the divalent metal in the divalent metal/polyion liquid-alkenyl resin particles is 0.1-5 wt%, and the content of the polyion liquid is 1-20 wt%.
Preferably, the particle size of the divalent metal is 20-500 nm, the particle size of the divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, and the D50 is 500-1500 nm.
Preferably, the polyionic liquid comprises an imidazole polyionic liquid or a quaternary phosphonium polyionic liquid; preferably imidazole-based polyionic liquids.
Preferably, the quaternary phosphine polyionic liquid comprises poly (p-vinylbenzyl-trialkyl quaternary phosphine hexafluorophosphate), poly (p-vinylbenzyl-trialkyl quaternary phosphine tetrafluoroborate), and poly (p-vinylbenzyl-trialkyl quaternary phosphine bistrifluoromethanesulfonylimide).
Preferably, the imidazole-based polyionic liquid has a structure of
Figure BDA0003414396200000031
a is 0-20, m is 10-5000, n is 10-5000, and X is BF4、PF6Or TFSI; or the imidazole polyion liquid has the structure of
Figure BDA0003414396200000032
n 10-5000, TFSI may be replaced by BF4Or PF6。
Preferably, the crosslinking agent comprises one or more of polyamide, diethylaminopropylamine, diphenylmethane crosslinking agent, toluyl peroxide, ketone peroxide, maleimide, carbamate and melamine resin.
Preferably, the dispersing agent comprises polyvinyl alcohol, polyvinylpyrrolidone, tricalcium phosphate, polyacrylic acid, dextrin and polyethylene glycol, the leveling agent comprises one or more of carboxymethyl cellulose, carboxyethyl cellulose and butyl cellulose, and/or
The defoaming agent comprises polyethylene wax APP230F, polyether defoaming agent, and/or
The flame retardant comprises magnesium hydroxide and aluminum hydroxide.
In another aspect of the present invention, a method for preparing a fireproof powder coating is provided, which comprises the following steps:
s1, preparation of divalent metal/polyion liquid-alkenyl resin particles: placing a monomer, divalent metal powder, an initiator, a surfactant, part of polyion liquid and a solvent of the alkenyl resin in a closed drying reactor, carrying out polymerization reaction for 4-10 h at a constant temperature of 50-80 ℃, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles;
s2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate, a curing agent and an auxiliary agent, and stirring at a high speed and then at a low speed to completely mix and react the materials;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
According to the invention, the monomer of the alkenyl resin, the divalent metal powder and the polyionic liquid are subjected to in-situ polymerization together, and the polyionic liquid and the alkenyl resin are coated on the surface of the divalent metal, so that the agglomeration phenomenon of the divalent metal powder can be improved, the problems of uneven distribution of metal particles in a resin material, large molecule agglomeration and poor modification effect are solved, and the electrical property and wear resistance of the coating can be effectively improved; and the polyion liquid and the resin material form a staggered complex structure, so that the divalent metal can be coated and modified, the structure of the resin material can be improved and repaired, and the structural strength of the resin material is improved. And then, crosslinking divalent metal/polyion liquid-alkenyl resin particles, polyion liquid and the like, wherein the polyion liquid not only promotes the curing of the alkenyl resin, but also can be used as a toughening agent to improve the comprehensive performance of the alkenyl resin.
Preferably, the initiator in step S1 includes one or more of azo initiator, peroxide initiator and redox initiator, the surfactant is anionic surfactant, and the solvent is cyclohexane.
Preferably, in step S1, the monomer of the alkenyl resin, the divalent metal powder, and a part of the polyionic liquid are mixed with a part of the solvent and dispersed for a period of time to form a dispersion, the surfactant and the rest of the solvent are mixed to form a mixture, and the dispersion, the mixture and the initiator are mixed to form a reaction solution, and then the reaction solution is placed in a sealed dry reactor.
Preferably, the mass concentration of the monomer of the alkenyl resin in the reaction liquid is 20-30 wt%, and the mass concentration of the surfactant is 1-5 wt%.
Preferably, the initiator is added in an amount of 1 to 5 wt% based on the monomer of the alkenyl resin in step S1.
Preferably, the temperature of the mixing reaction in the step S2 is 50-80 ℃, the high-speed stirring speed is 600-1000 r/min, and the low-speed stirring speed is 300-600 r/min.
The invention can obtain at least one of the following beneficial effects:
according to the invention, the monomer of the alkenyl resin, the divalent metal powder and the polyionic liquid are subjected to in-situ polymerization together, and the polyionic liquid and the alkenyl resin are coated on the surface of the divalent metal, so that the agglomeration phenomenon of the divalent metal powder can be improved, the problems of uneven distribution of metal particles in a resin material, large molecule agglomeration and poor modification effect are solved, and the electrical performance of the coating can be effectively improved; and the polyion liquid and the resin material form a staggered complex structure, so that the divalent metal can be coated and modified, the structure of the resin material can be improved and repaired, and the structural strength of the resin material is improved. Then, crosslinking divalent metal/polyion liquid-alkenyl resin particles, polyion liquid and the like, wherein the polyion liquid not only promotes the curing of the alkenyl resin, but also can be used as a toughening agent to improve the performances of the alkenyl resin and the obtained coating; with hydrophobic SiO2-TiO2The composite gel, ammonium dihydrogen phosphate, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride and other raw materials are compositely crosslinked, and the comprehensive performance of the coating is greatly improved by utilizing the characteristic synergistic effect of the raw materials.
The coating film obtained by the coating disclosed by the invention has excellent corrosion resistance, high surface resistance and high toughness, and can adapt to various service environments.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
In the following examples, hydrophobic SiO2-TiO2The preparation method of the composite gel comprises the following steps:
mixing ethyl orthosilicate, ethylene-bis (octadecyl dimethyl ammonium chloride), ethanol and water in proportion, and stirring at 55 deg.C for 6 hr to obtain Gemini type SiO2And (5) dissolving the sol, and standing for later use. Mixing tetra-n-butyl titanate and ethanol, slowly adding the mixed solution of hydrochloric acid and water dropwise under stirring, and continuously stirring for 30min to obtain TiO2And (5) dissolving the sol, and standing for later use.
Then a certain amount of Gemini type SiO is taken2Uniformly mixing the sol and absolute ethyl alcohol, and slowly dripping TiO with a proper proportion under the condition of continuous stirring2Dissolving the sol, then dropwise adding a certain amount of deionized water, and continuously stirring for 0.5h at room temperature after dropwise adding to obtain the Gemini type SiO2/TiO2And (4) compounding the sol. The ratio of silicon to titanium in the composite sol is 4:1, and the concentration is 0.3 mol/L.
1H,1H,2H, 2H-perfluorooctyltriethoxysilane (1/5 gel mass) was added to SiO2-TiO2Stirring the composite gel for 1 hour at room temperature to obtain hydrophobic SiO2-TiO2And (4) compounding the gel.
Example 1
A fireproof powder coating comprises the following raw materials in parts by weight: 40 parts of divalent metal/polyion liquid-alkenyl resin particles, 2 parts of polyion liquid, 8 parts of polyamide and hydrophobic SiO2-TiO215 parts of composite gel, 8 parts of ammonium dihydrogen phosphate, 3 parts of magnesium oxide, 3 parts of montmorillonite, 2 parts of barium sulfate whisker, 1 part of silicon nitride, 2 parts of 704 curing agent and 3 parts of polyvinyl alcohol, wherein the monomer of the alkenyl resinThe high-performance composite material comprises styrene and hydroxyethyl methacrylate, divalent metal is titanium oxide and copper oxide with equal mass, the particle size of divalent metal powder is 20-500 nm, the particle size of divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, D50 is 500-1500 nm, the content of the divalent metal is 0.25 wt%, and the content of polyion liquid is 15 wt%. The polyion liquid has the structure of
Figure BDA0003414396200000071
a is 0, m is 10-5000, n is 10-5000, and X is TFSI.
A preparation method of a fireproof powder coating comprises the following steps:
s1, preparation of an alkenyl resin/divalent metal powder core-shell structure:
mixing and dispersing a monomer of alkenyl resin, divalent metal powder and polyion liquid with a solvent of 4/5 for a period of time to prepare a dispersion liquid, mixing polyvinyl alcohol and the rest of the solvent to prepare a mixed liquid, mixing the dispersion liquid, the mixed liquid and an initiator azobisisobutyronitrile to obtain a reaction liquid, then placing the reaction liquid in a closed drying reactor, carrying out constant-temperature polymerization reaction at 50 ℃ for 10 hours, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles; wherein the addition amount of the initiator is 1.5 wt% of the monomer of the alkenyl resin, and the solvent is water; the mass concentration of the monomer of the alkenyl resin in the reaction liquid was 20 wt%, and the mass concentration of the surfactant was 1 wt%.
S2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, the cross-linking agent and the hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate and an accelerant, stirring at the rotating speed of 1000r/min at 50 ℃, and then stirring at the rotating speed of 600r/min until the reaction is finished;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
Example 2
A fireproof powder coating comprises the following raw materials in parts by weight: divalent metal/polyion liquid80 parts of bulk-alkenyl resin particles, 8 parts of polyion liquid, 10 parts of diethylaminopropylamine, 10 parts of carbamate and hydrophobic SiO2-TiO28 parts of composite gel, 15 parts of ammonium dihydrogen phosphate, 10 parts of magnesium oxide, 10 parts of montmorillonite, 8 parts of barium sulfate whisker, 5 parts of silicon nitride, 8 parts of HDI tripolymer, 1.5 parts of polyvinylpyrrolidone, 1.5 parts of tricalcium phosphate, 3 parts of magnesium hydroxide and 3 parts of aluminum hydroxide, wherein divalent metal is iron oxide and zinc oxide with equal mass, and monomers of alkenyl resin comprise butyl methacrylate, butyl acrylate and hydroxyethyl acrylate with equal mass. The content of the divalent metal in the divalent metal/polyion liquid-alkenyl resin particles is 4.5 wt%, the particle size of the divalent metal powder is 20-500 nm, the particle size of the divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, and D50 is 500-1500 nm. The structural formula of the polyion liquid is
Figure BDA0003414396200000081
a is 12, m is 10-5000, n is 10-5000, and X is BF4。
A preparation method of a fireproof powder coating comprises the following steps:
s1, preparation of an alkenyl resin/divalent metal powder core-shell structure:
mixing a monomer of alkenyl resin, divalent metal powder, polyion liquid and a half solvent, dispersing for a period of time to prepare dispersion liquid, mixing nonylphenol alkylphenol polyoxyethylene ether and the rest solvent to prepare mixed liquid, mixing the dispersion liquid, the mixed liquid and an initiator dimethyl azodiisobutyrate to obtain reaction liquid, putting the reaction liquid into a closed drying reactor, carrying out constant-temperature polymerization reaction at 80 ℃ for 4 hours, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles; the addition amount of the initiator is 4.5 wt% of the monomer of the alkenyl resin, and the solvent is water; the mass concentration of the monomer of the alkenyl resin in the reaction liquid was 30 wt%, and the mass concentration of the surfactant was 5 wt%.
S2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Composite gel, magnesium oxide, montmorillonite and sulfuric acidMixing barium whisker, silicon nitride, ammonium dihydrogen phosphate and an accelerant, stirring at the rotating speed of 600r/min at the temperature of 80 ℃, and then stirring at the rotating speed of 300r/min until the reaction is finished;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
Example 3
A fireproof powder coating comprises the following raw materials in parts by weight: 50 parts of divalent metal/polyion liquid-alkenyl resin particles, 6 parts of polyion liquid, 5 parts of diethylaminopropylamine, 5 parts of melamine resin and hydrophobic SiO2-TiO210 parts of composite gel, 10 parts of ammonium dihydrogen phosphate, 5 parts of magnesium oxide, 5 parts of montmorillonite, 4 parts of barium sulfate whisker, 2 parts of silicon nitride, 3.5 parts of 705 curing agent, 1 part of carboxymethyl cellulose, 1 part of tricalcium phosphate, 2 parts of polyethylene glycol and 230F 1 parts of polyethylene wax, wherein the auxiliary agent comprises one or more of a dispersing agent, a leveling agent, an antifoaming agent and a flame retardant. The divalent metal comprises equal mass of calcium carbonate and barium sulfate. The monomer of the alkenyl resin comprises methyl acrylate and hydroxyethyl methacrylate with equal mass. The content of the divalent metal in the divalent metal/polyion liquid-alkenyl resin particles is 1.5 wt%, the particle size of the divalent metal powder is 20-500 nm, the particle size of the divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, and D50 is 500-1500 nm. The structural formula of the polyion liquid is
Figure BDA0003414396200000091
a is 8, m is 10-5000, n is 10-5000, and X is PF6。
A preparation method of a fireproof powder coating comprises the following steps:
s1, preparation of an alkenyl resin/divalent metal powder core-shell structure:
mixing a monomer of the alkenyl resin, divalent metal powder, polyion liquid and a half solvent, dispersing for a period of time to prepare dispersion liquid, mixing sodium dodecyl benzene sulfonate and the rest solvent to prepare mixed liquid, mixing the dispersion liquid, the mixed liquid and an initiator potassium persulfate to obtain reaction liquid, then placing the reaction liquid in a closed drying reactor, carrying out constant-temperature polymerization reaction for 8 hours at 60 ℃, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles; the addition amount of the initiator is 2 wt% of the monomer of the alkenyl resin, and the solvent is water; the mass concentration of the monomer of the alkenyl resin in the reaction liquid was 22.5 wt%, and the mass concentration of the surfactant was 2 wt%.
S2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate and an accelerant, uniformly stirring at the rotating speed of 800r/min at the temperature of 60 ℃, and then stirring at the rotating speed of 400r/min until the reaction is finished;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
Example 4
A fireproof powder coating comprises the following raw materials in parts by weight: 60 parts of divalent metal/polyion liquid-alkenyl resin particles, 5 parts of polyion liquid, 8 parts of diethylaminopropylamine, 7 parts of ketone peroxide and hydrophobic SiO2-TiO212 parts of composite gel, 12 parts of ammonium dihydrogen phosphate, 6 parts of magnesium oxide, 6 parts of montmorillonite, 5 parts of barium sulfate whisker, 3 parts of silicon nitride, 2.5 parts of methylimidazole, 2.5 parts of HDI trimer, 2 parts of dextrin, 2 parts of carboxyethyl cellulose, 230F 1 parts of polyethylene wax, 2 parts of magnesium hydroxide and 1 part of aluminum hydroxide, wherein the divalent metal comprises copper oxide, zinc oxide and magnesium oxide with equal mass, and the monomer of the alkenyl resin comprises one or more of styrene, methyl methacrylate and hydroxyethyl acrylate. The content of the divalent metal in the divalent metal/polyion liquid-alkenyl resin particles is 2.5 wt%, the particle size of the divalent metal powder is 20-500 nm, the particle size of the divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, and D50 is 500-1500 nm. The polyionic liquid is Poly (BVim)][HIm][TFSI]Structural formula is
Figure BDA0003414396200000101
n＝10-5000。
A preparation method of a fireproof powder coating comprises the following steps:
s1, preparation of an alkenyl resin/divalent metal powder core-shell structure:
mixing and dispersing a monomer, divalent metal powder and polyion liquid of alkenyl resin with 2/3 solvent for a period of time to prepare dispersion liquid, mixing sodium lignosulfonate with the rest solvent to prepare mixed liquid, mixing the dispersion liquid, the mixed liquid and an initiator azobisisoheptonitrile to obtain reaction liquid, then placing the reaction liquid in a sealed drying reactor, carrying out polymerization reaction at the constant temperature of 70 ℃ for 7 hours, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles; the addition amount of the initiator is 3 wt% of the monomer of the alkenyl resin, the surfactant is an anionic surfactant, and the solvent is water; the mass concentration of the monomer of the alkenyl resin in the reaction liquid was 25 wt%, and the mass concentration of the surfactant was 3 wt%.
S2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate and an accelerant, uniformly stirring at the rotating speed of 800r/min at 70 ℃, and then stirring at the rotating speed of 450r/min until the reaction is finished;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
Example 5
A fireproof powder coating comprises the following raw materials in parts by weight: 70 parts of divalent metal/polyion liquid-alkenyl resin particles, 6.5 parts of polyion liquid, 8 parts of polyamide, 8 parts of maleimide and hydrophobic SiO2-TiO213 parts of composite gel, 11 parts of ammonium dihydrogen phosphate, 8 parts of magnesium oxide, 7 parts of montmorillonite, 6 parts of barium sulfate whisker, 3.5 parts of silicon nitride, 3 parts of 2-phenylimidazole, 3 parts of HDI trimer, 2 parts of dextrin, 1 part of carboxymethyl cellulose, 2.5 parts of magnesium hydroxide and 2.5 parts of aluminum hydroxide, wherein divalent metal comprises titanium oxide, copper oxide, magnesium oxide and calcium carbonate with equal mass, monomers of alkenyl resin comprise styrene, butyl acrylate, hydroxyethyl methacrylate with equal mass, and divalent metal/polyion liquid-alkenyl resin particlesThe content of the divalent metal in the particles is 3.2 wt%, the particle size of the divalent metal powder is 20-500 nm, the particle size of the divalent metal/polyion liquid-alkenyl resin particles is 100-2000 nm, and D50 is 500-1500 nm. The polyionic liquid is poly (p-vinylbenzyl-trialkyl quaternary phosphonium hexafluorophosphate).
A preparation method of a fireproof powder coating comprises the following steps:
s1, preparation of an alkenyl resin/divalent metal powder core-shell structure:
mixing and dispersing a monomer, divalent metal powder and polyion liquid of alkenyl resin with half water for a period of time to prepare dispersion liquid, mixing nonylphenol alkylphenol polyoxyethylene ether with the rest water to prepare mixed liquid, mixing the dispersion liquid, the mixed liquid and initiator benzoyl peroxide tert-butyl ester to obtain reaction liquid, then placing the reaction liquid into a closed drying reactor, carrying out polymerization reaction at the constant temperature of 65 ℃ for 7 hours, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles; the addition amount of the initiator is 3.5 wt% of the monomer of the alkenyl resin, the mass concentration of the monomer of the alkenyl resin in the reaction liquid is 27.2 wt%, and the mass concentration of the surfactant is 3.8 wt%;
s2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate and an accelerant, uniformly stirring at 65 ℃ at the rotating speed of 900r/min, and then stirring at the rotating speed of 500r/min until the reaction is finished;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
Comparative example 1
The divalent metal powder was added in step S2, the rest being the same as in example 1.
Comparative example 2
Hydrophobic SiO2-TiO2The composite gel is replaced by equal amount of SiO2And TiO2Otherwise, the same procedure as in example 1 was repeated.
Comparative example 3
The polyionic liquid in steps S1 and S2 was removed, as in example 1.
Comparative example 4
The polyionic liquid is added in its entirety in step S2, as in example 1.
The powder coatings obtained in examples 1 to 5 and comparative examples 1 to 4 were coated on test plates formed of cold-rolled steel sheets having a thickness of 0.6mm and subjected to titanium oxide phosphate treatment so that the film thickness after baking was 30 μm, baked at 170 ℃ for 1 hour, and then cooled to room temperature, to thereby obtain coating film samples. The coating film was then tested for properties and the results are shown in Table 1.
1. Bending strength
The test was carried out according to the regulations of GB/6742-1986.
2. Corrosion resistance
Salt spray tests were carried out as specified in GB/T17711991.
3. Surface resistance
And placing the surface resistance tester on the surface of the sample for testing.
TABLE 1
Bending strength Corrosion resistance Surface resistance
Example 1 2mm >2500h 7.6×1010Ω
Example 2 2mm >2500h 9.3×1010Ω
Example 3 2mm >2500h 1.1×1011Ω
Example 4 2mm >2500h 5.9×1010Ω
Example 5 2mm >2500h 8.7×1010Ω
Comparative example 1 3mm >2100h 3.8×108Ω
Comparative example 2 4mm >1700h 7.2×109Ω
Comparative example 3 5mm >1500h 4.5×109Ω
Comparative example 4 4mm >2000h 2.3×1010Ω
As can be seen from the data in Table 1, the divalent metal powder and the polyion liquid have certain effects on the bending strength, corrosion resistance and surface resistance of the coating film, particularly the divalent metal powder (comparative example 1) has the greatest effect on the surface resistance, the divalent metal powder improves the insulation and antistatic properties of the coating film, and the hydrophobic SiO2-TiO2The composite gel (comparative example 2) and polyionic liquid (comparative example 3) have a large effect on corrosion resistance and bending strength, and the manner of bonding polyionic liquid to alkenyl resin (comparative example 4) has a large effect on bending strength. The coating film prepared by the coating has excellent bending strength, corrosion resistance and high surface resistance.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (10)

1. The fireproof powder coating is characterized by comprising the following raw materials in parts by weight: 40-80 parts of divalent metal/polyion liquid-alkenyl resin particles, 2-8 parts of polyion liquid, 8-20 parts of cross-linking agent and hydrophobic SiO2-TiO28-15 parts of composite gel, 8-15 parts of ammonium dihydrogen phosphate, 3-10 parts of magnesium oxide, 3-10 parts of montmorillonite, 2-8 parts of barium sulfate whisker, 1-5 parts of silicon nitride, 2-8 parts of curing agent and 3-10 parts of auxiliary agent, wherein the auxiliary agent comprises a dispersing agent and a flatting agentOne or more of defoaming agent and flame retardant.
2. A fire-resistant powder coating according to claim 1, wherein the divalent metal comprises one or more of titanium oxide, copper oxide, iron oxide, zinc oxide, magnesium oxide, calcium carbonate, barium sulfate; the monomer of the alkenyl resin comprises one or more of styrene, butyl methacrylate, butyl acrylate, methyl methacrylate and methyl acrylate, and one or more of hydroxyethyl methacrylate and hydroxyethyl acrylate.
3. A fire-retardant powder coating according to claim 1, wherein the divalent metal/polyion liquid-alkenyl resin particles contain the divalent metal in an amount of 0.1 to 5 wt% and the polyion liquid in an amount of 1 to 15 wt%.
4. The fireproof powder coating of claim 1, wherein the divalent metal has a particle size of 20-500 nm, the divalent metal/polyion liquid-alkenyl resin particles have a particle size of 100-2000 nm, and D50 is 500-1500 nm.
5. A fire-retardant powder coating according to claim 1, wherein said polyionic liquid comprises an imidazole-based polyionic liquid or a quaternary phosphine-based polyionic liquid.
6. A fire-retardant powder coating according to claim 1, wherein said cross-linking agent comprises one or more of polyamide, diethylaminopropylamine, diphenylmethane cross-linking agent, toluyl peroxide, ketone peroxide, maleimide, urethane, and melamine resin.
7. A fire-retardant powder coating according to claim 1, wherein said dispersing agent comprises polyvinyl alcohol, polyvinylpyrrolidone, tricalcium phosphate, polyacrylic acid, dextrin, polyethylene glycol, and said leveling agent comprises one or more of carboxymethyl cellulose, carboxyethyl cellulose, butyl cellulose, and/or
The defoaming agent comprises polyethylene wax APP230F, polyether defoaming agent, and/or
The flame retardant comprises magnesium hydroxide and aluminum hydroxide.
8. The preparation method of the fireproof powder coating is characterized by comprising the following steps:
s1, preparation of divalent metal/polyion liquid-alkenyl resin particles: placing a monomer, divalent metal powder, an initiator, a surfactant, part of polyion liquid and a solvent of the alkenyl resin in a closed drying reactor, carrying out polymerization reaction for 4-10 h at a constant temperature of 50-80 ℃, adding an ethanol solution of 5% HCl to terminate polymerization, filtering, washing and drying to obtain divalent metal/polyion liquid-alkenyl resin particles;
s2, mixing the divalent metal/polyion liquid-alkenyl resin particles, the residual polyion liquid, a cross-linking agent and hydrophobic SiO2-TiO2Mixing the composite gel, magnesium oxide, montmorillonite, barium sulfate whisker, silicon nitride, ammonium dihydrogen phosphate, a curing agent and an auxiliary agent, and stirring at a high speed and then at a low speed to completely mix and react the materials;
and S3, cooling the reacted materials, rolling and coarsely crushing, and then grinding and refining to obtain the fireproof powder coating.
9. The method according to claim 8, wherein in step S1, the monomer of the alkenyl resin, the divalent metal powder, and a part of the polyionic liquid are mixed with a part of the solvent and dispersed for a period of time to form a dispersion, the surfactant and the rest of the solvent are mixed to form a mixture, and the mixture, and the initiator are mixed to form a reaction solution, and then the reaction solution is placed in a sealed dry reactor.
10. The method of claim 8, wherein the temperature of the mixing reaction in step S2 is 50-80 ℃, the rotation speed of the high-speed stirring is 600-1000 r/min, and the rotation speed of the low-speed stirring is 300-600 r/min.
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