CN111662620A - Preparation method of powder coating for fireproof door - Google Patents
Preparation method of powder coating for fireproof door Download PDFInfo
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- CN111662620A CN111662620A CN202010638376.0A CN202010638376A CN111662620A CN 111662620 A CN111662620 A CN 111662620A CN 202010638376 A CN202010638376 A CN 202010638376A CN 111662620 A CN111662620 A CN 111662620A
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/48—Stabilisers against degradation by oxygen, light or heat
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Abstract
The invention discloses a preparation method of powder coating for a fireproof door; relates to the technical field of paint spraying, and comprises the following steps: (1) preparing composite silicon micro powder particles; (2) preparing diatomite particle-loaded benzoin; (3) mixing the raw materials; the powder coating for the fireproof door prepared by the method has excellent impact resistance, and the occasions where the fireproof door is damaged by impact are large, so that the fireproof door can be better protected by using the powder coating for the fireproof door prepared by the method, the surface of the coating can be kept from being damaged when the fireproof door is impacted for a certain time, and the service life of the powder coating is prolonged.
Description
Technical Field
The invention belongs to the technical field of paint spraying, and particularly relates to a preparation method of powder paint for a fireproof door.
Background
The fire department economic department designates an approved laboratory, the fire door fire resistance test method is tested to be qualified according to the national standard GB _12955 once 2008 of the new fire door, which is implemented from 1 month and 1 day in 2009, and the fire door is called as a fire door by obtaining the certification and login certificate and the authorized identifier of the ministry of economy standard inspection bureau. Fire rated doors, as defined by the NFPA and IBC specifications in the united states, are "any combination of fire rated door leaves, jambs, hardware and other fittings that together provide some degree of fire protection to an opening.
A fire door is a door that can meet the requirements of fire stability, integrity and thermal insulation within a certain period of time. It is a fire-proof partition with certain fire resistance, which is arranged in fire-proof subareas, evacuation staircases, vertical shafts and the like.
The fireproof door has the functions of a common door, has the functions of preventing the fire from spreading and the smoke from diffusing, and can prevent the fire from spreading within a certain time to ensure the evacuation of people.
In order to improve the protection of the fire door, the surface of the fire door is usually coated with a coating to prevent the fire door from being corroded by corrosive factors in the air, so that the fire door is rotten and cannot be used continuously.
The prior art is as follows: "application publication number is: CN 108715718A, a fireproof door coating, the application discloses a fireproof door coating, which comprises, by weight, 122 parts of butyl acetate, 58 parts of bamboo charcoal fiber, 26 parts of sodium hydroxide, 160 parts of sodium polyacrylate, 79 parts of fluorocarbon emulsion, 99 parts of polyether modified polysiloxane, 69 parts of dibutyl phosphate, 37 parts of tetrachloro-m-phthalonitrile, 48 parts of sodium sulfite and 138 parts of cyclohexanone. Therefore, the coating has a reasonable formula, has high antirust performance, corrosion resistance and heat insulation performance, and is beneficial to environmental protection, although the coating has the antirust function, the flexibility and impact resistance of the coating are general, after the coating is applied to the surface of a fireproof door, the fireproof door can be bent due to small-amplitude impact, the coating can be directly broken, and the fireproof door cannot be continuously protected, so that the technical problem to be solved is how to further improve the mechanical performance of the fireproof door coating.
Disclosure of Invention
The invention aims to provide a preparation method of a powder coating for a fireproof door, which aims to overcome the defects in the prior art.
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78-85 ℃, keeping the temperature, stirring at a high speed for reaction for 30-40min, then filtering, washing, drying to constant weight, calcining for 15-18min at 400-500 ℃, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles;
(2) preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3-4 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water;
(3) mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder.
The mass fraction of the antimony potassium tartrate solution is 6-8%;
the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution.
The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1-3:45-50: 6-10.
The mass fraction of the benzoin in the ethanol dispersion liquid is 5-7%;
the mass fraction of ethanol is 40%.
The weight parts of the calcined diatomite particles, the ethanol dispersion liquid and the cardanol are 14-16: 18-22: 0.5-0.9.
The preparation method of the calcined diatomite particles comprises the following steps:
adding diatomite into a resistance furnace, calcining for 1 hour at the temperature of 500-540 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder;
the average particle size of the diatomaceous earth after sieving was 20 μm.
The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (12-15: 4-5): 50-60: 4-5: 0.2-0.4:10-12.
The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1.
The curing agent is a beta-hydroxyalkylamide.
The leveling agent is polydimethylsiloxane.
The technical scheme adopted by the invention is as follows:
the preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
The average particle size of the powder coating for the fireproof door is 30 micrometers;
the particle size distribution of the powder coating can influence the leveling property, the powdering rate and the recovery rate of the coating. Generally, the smaller the particle size of the coating, the more favorable the leveling property during curing, and the smoother and smoother the appearance of the coating film. Meanwhile, the thickness of the coating can be reduced due to small particle size of the coating particles, a larger area can be coated by the coating with the same quality, but the particle size of the powder coating is not smaller as well as better. The powder with small particle size has poor electrification property, so that the powdering rate is reduced, and therefore, a great deal of experimental research shows that the coating obtained by the fireproof door powder coating has the best performance when the average particle size is 30 mu m.
According to the invention, beta-hydroxyalkylamide is used as a curing agent of the fireproof door powder coating, but the high-temperature yellowing resistance of the powder coating is poor due to the naked N atom on the main chain of the beta-hydroxyalkylamide molecule.
According to the invention, the polyester resin is adopted as the matrix resin, the melt viscosity of the powder coating is increased by adjusting and controlling the dosage of the polyester resin, the molecular motion speed and the curing rate are improved by the synergistic effect of the polyester resin and other components, the curing time is reduced, and the mechanical property of the coating is improved.
Has the advantages that:
the powder coating for the fireproof door prepared by the method has excellent impact resistance, and the occasions where the fireproof door is damaged by impact are large, so that the fireproof door can be better protected by using the powder coating for the fireproof door prepared by the method, the surface of the coating can be kept from being damaged when the fireproof door is impacted for a certain time, and the service life of the powder coating is prolonged.
Detailed Description
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78-85 ℃, keeping the temperature, stirring at a high speed for reaction for 30-40min, then filtering, washing, drying to constant weight, calcining for 15-18min at 400-500 ℃, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles;
antimony Potassium Tartrate (L-Antimony Potassium tantrate) is a colorless transparent crystalline or white powder. The relative density was 2.607. It is slowly weathered in the air. The water of crystallization is lost at 100 ℃. Dissolving in water and glycerol. It is insoluble in alcohol. The aqueous solution is weakly alkaline. When tannic acid is encountered, white precipitate is generated. Molecular formula C8H4K2O12Sb2And the molecular weight is 613.82700.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3-4 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water;
diatomite:
the chemical composition of diatomite is mainly SiO2, and contains small amount of Al2O3, Fe2O3, CaO, MgO, etc. and organic matter, and the density of diatomite is 1.9-2.3 g/cm3Bulk density of 0.34-0.65 g/cm3Performing high-temperature distillation on the pulp with the specific surface area of 40-65 m/g and the pore volume of 0.45-0.98 cm/g, wherein the water absorption is 2-4 times of the volume of the pulp, and the melting point of 1650-1750 ℃;
(3) mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder.
The mass fraction of the antimony potassium tartrate solution is 6-8%;
the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution.
The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1-3:45-50: 6-10.
The mass fraction of the benzoin in the ethanol dispersion liquid is 5-7%;
the mass fraction of ethanol is 40%.
The weight parts of the calcined diatomite particles, the ethanol dispersion liquid and the cardanol are 14-16: 18-22: 0.5-0.9.
The preparation method of the calcined diatomite particles comprises the following steps:
adding diatomite into a resistance furnace, calcining for 1 hour at the temperature of 500-540 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder;
the average particle size of the diatomaceous earth after sieving was 20 μm.
The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (12-15: 4-5): 50-60: 4-5: 0.2-0.4:10-12.
The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1.
The curing agent is a beta-hydroxyalkylamide.
The leveling agent is polydimethylsiloxane.
The dimethyl silicone oil in the chemical state of the polydimethylsiloxane is colorless or light yellow liquid, is tasteless and high in transparency, has heat resistance, cold resistance, small viscosity change along with temperature, waterproofness, small surface tension and heat conductivity, has the heat conductivity coefficient of 0.134-0.159W/M.K and the light transmittance of 100 percent, is nontoxic and tasteless, and has physiological inertia and good chemical stability. Good electric insulation, weather resistance and hydrophobicity, and high shear resistance, and can be used for a long time at the temperature of between 50 ℃ below zero and 200 ℃.
The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78 ℃, keeping the temperature, stirring at a high speed for reaction for 30min, then filtering, washing, drying to constant weight, calcining at 400 ℃ for 15min, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 6 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1:45: 6. The mass fraction of the benzoin in the ethanol dispersion liquid is 5%; the mass fraction of ethanol is 40%.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water; the weight ratio of the calcined diatomite particles to the ethanol dispersion liquid to the cardanol is (14: 18): 0.5. the preparation method of the calcined diatomite particles comprises the following steps: adding diatomite into a resistance furnace, calcining for 1 hour at 500 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder; the average particle size of the diatomaceous earth after sieving was 20 μm.
(3) Mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder. The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (12: 4): 50: 4: 0.2:10. The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
Example 2
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 85 ℃, keeping the temperature, stirring at a high speed for reaction for 40min, then filtering, washing, drying to constant weight, then calcining for 18min at 500 ℃, then naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 8 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 3:50: 10. The mass fraction of the benzoin in the ethanol dispersion liquid is 7%; the mass fraction of ethanol is 40%.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 4 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water; the weight ratio of the calcined diatomite particles to the ethanol dispersion liquid to the cardanol is 16: 22: 0.9. the preparation method of the calcined diatomite particles comprises the following steps: adding diatomite into a resistance furnace, calcining for 1 hour at 540 ℃, naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder; the average particle size of the diatomaceous earth after sieving was 20 μm.
(3) Mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder. The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (15: 5): 60: 5: 0.4:12. The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
Example 3
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into a potassium antimony tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 81 ℃, keeping the temperature, stirring at a high speed for reaction for 35min, then filtering, washing, drying to constant weight, calcining for 16min at 420 ℃, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 7 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 2:46: 8. The mass fraction of the benzoin in the ethanol dispersion liquid is 6%; the mass fraction of ethanol is 40%.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3.5 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water; the weight parts of the calcined diatomite particles, the ethanol dispersion liquid and the cardanol are (15: 20): 0.6. the preparation method of the calcined diatomite particles comprises the following steps: adding diatomite into a resistance furnace, calcining for 1 hour at 520 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder; the average particle size of the diatomaceous earth after sieving was 20 μm.
(3) Mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder. The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is 13.5: 4.5: 55: 4.5: 0.3:11. The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
Example 4
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78 ℃, keeping the temperature, stirring at a high speed for reaction for 40min, then filtering, washing, drying to constant weight, calcining at 400 ℃ for 15min, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 8 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1:45: 10. The mass fraction of the benzoin in the ethanol dispersion liquid is 5%; the mass fraction of ethanol is 40%.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water; the weight ratio of the calcined diatomite particles to the ethanol dispersion liquid to the cardanol is 16: 18: 0.9. the preparation method of the calcined diatomite particles comprises the following steps: adding diatomite into a resistance furnace, calcining for 1 hour at 500 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder; the average particle size of the diatomaceous earth after sieving was 20 μm.
(3) Mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder. The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (15: 5): 60: 4: 0.2:10. The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
Example 5
A preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into a potassium antimony tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 85 ℃, keeping the temperature, stirring at a high speed for reaction for 35min, then filtering, washing, drying to constant weight, calcining for 16min at 450 ℃, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 8 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1:50: 10. The mass fraction of the benzoin in the ethanol dispersion liquid is 6%; the mass fraction of ethanol is 40%.
(2) Preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water; the weight parts of the calcined diatomite particles, the ethanol dispersion liquid and the cardanol are (15: 21): 0.7. the preparation method of the calcined diatomite particles comprises the following steps: adding diatomite into a resistance furnace, calcining for 1 hour at 520 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder; the average particle size of the diatomaceous earth after sieving was 20 μm.
(3) Mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder. The weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (12: 4): 60: 4: 0.4:10. The weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min at the microwave power of 500W, cooling the reaction solution to room temperature, gradually precipitating a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin.
Uniformly coating the prepared powder coating on a tin plate with the size of 60mm multiplied by 150 mm multiplied by 0.5 mm by using an electrostatic spray gun respectively, controlling the film thickness to be 50 mu m, placing the powder coating into a curing furnace for baking and curing after spraying, and taking out a sample plate after heat preservation for 8min at 180 ℃. The sample plate is placed in a constant temperature and humidity environment with the temperature of 23 +/-2 ℃ and the relative humidity of 50 +/-5 percent, and various performances are tested according to the standard.
The test was carried out with a coating impact tester (QCJ) according to GB/T1732-93, "determination of impact resistance of paint films". TABLE 1
| Impact resistance/(kg. cm) | |
| Example 1 | 52.3 |
| Example 2 | 52.8 |
| Example 3 | 53.5 |
| Example 4 | 54.1 |
| Example 5 | 54.3 |
| Control group | 32.6 |
Control group: the application publication numbers are: CN 108715718A;
as can be seen from Table 1, the powder coating for fire doors prepared by the method of the present invention has excellent impact resistance, and the fire doors are damaged by impact in a large number of occasions, so that the powder coating for fire doors prepared by the method of the present invention can protect the fire doors better, and when the fire doors are subjected to a certain impact, the surface of the coating can be kept from being damaged, thereby prolonging the service life of the powder coating.
Referring to a test method of a 7 th part bending test of GB/T13448-2006 standard, a T-shaped bending tester is adopted for testing;
TABLE 2
| 0T bend | |
| Example 1 | Without cracking |
| Example 2 | Without cracking |
| Example 3 | Without cracking |
| Example 4 | Without cracking |
| Example 5 | Without cracking |
| Control group | Cracking of |
Control group: the application publication numbers are: CN 108715718A;
as shown in Table 2, the surface coating for the fireproof door prepared by the method disclosed by the invention has excellent mechanical properties, can better resist cracking, and is very suitable for the fireproof door.
With reference to ISO 8130-8: 1994 powder coating part 8: evaluation of the storage stability of thermosetting powder coatings Using an electric forced air drying Cabinet (WGL-125B):
TABLE 3
| Storage stability of [ (42 +/-1) DEG C, 7d] | |
| Example 1 | Without change |
| Example 2 | Without change |
| Example 3 | Without change |
| Example 4 | Without change |
| Example 5 | Without change |
| Comparative example 1 | Slightly compacted |
Comparative example 1: a preparation method of powder coating for a fireproof door comprises the following steps:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78 ℃, keeping the temperature, stirring at a high speed for reaction for 40min, then filtering, washing, drying to constant weight, calcining at 400 ℃ for 15min, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles; the mass fraction of the antimony potassium tartrate solution is 8 percent; the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution. The mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1:45: 10. The mass fraction of the benzoin in the ethanol dispersion liquid is 5%; the mass fraction of ethanol is 40%.
(2) Mixing raw materials:
and sequentially adding the composite silicon micro powder particles, the diatomite, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer to be uniformly stirred, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the silicon nano composite material. The weight ratio of the composite silicon micropowder particles, the diatomite, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler is (15: 5): 60: 4: 0.2:10. The curing agent is a beta-hydroxyalkylamide. The leveling agent is polydimethylsiloxane. The preparation method of benzoin comprises the following steps: adding 40mL of anhydrous ethanol and 20mL of distilled water into a reaction kettle, adding zeolite, immersing the zeolite into cold water, adding a certain amount of vitamin B1 into the reaction kettle, oscillating to dissolve the vitamin B, adding 50 mL of newly distilled benzaldehyde, oscillating and shaking uniformly to obtain a light yellow solution, adjusting the pH of the reaction solution to a certain value by using a sodium hydroxide solution, testing the pH of the system reaction solution by using a pH meter, after the adjustment is completed, carrying out microwave treatment for 10min, wherein the microwave power is 500W, cooling the reaction solution to room temperature, gradually separating out a solid, washing for multiple times by using a sodium bicarbonate solution and distilled water, recrystallizing, carrying out suction filtration, and drying to obtain a white powdery product, namely benzoin;
as can be seen from Table 3, the fireproof door powder coating prepared by the method provided by the invention has good storage stability, and the storage stability of the powder coating can be improved to a certain extent by adding diatomite to load benzoin.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the powder coating for the fireproof door is characterized by comprising the following steps of:
(1) preparing composite silicon micro powder particles:
dissolving antimony potassium tartrate in deionized water to obtain an antimony potassium tartrate solution;
dissolving ammonium bicarbonate in deionized water to obtain an ammonium bicarbonate solution;
dropwise adding an ammonium bicarbonate solution into an antimony potassium tartrate solution, then adding lignosulfonate and silicon micropowder, adjusting the temperature to 78-85 ℃, keeping the temperature, stirring at a high speed for reaction for 30-40min, then filtering, washing, drying to constant weight, calcining for 15-18min at 400-500 ℃, naturally cooling to room temperature, grinding and sieving to obtain composite silicon micropowder particles;
(2) preparing diatomite particle-loaded benzoin:
adding benzoin into an ethanol solution, and uniformly stirring to obtain an ethanol dispersion liquid;
adding the calcined diatomite particles into the ethanol dispersion liquid, stirring for 3-4 hours, then adding cardanol, continuing stirring for 1 hour, and then drying to remove ethanol and water;
(3) mixing raw materials:
adding the composite silicon micro powder particles, the diatomite particles loaded with benzoin, the polyester resin powder, the curing agent, the flatting agent and the inorganic filler into a stirrer in sequence, stirring uniformly, then carrying out melt extrusion in an extruder, cooling, tabletting, crushing and sieving to obtain the composite silicon micro powder.
2. The preparation method of the powder coating for the fire door according to claim 1, wherein the powder coating comprises the following steps: the mass fraction of the antimony potassium tartrate solution is 6-8%;
the molar ratio of ammonium bicarbonate to antimony potassium tartrate is 1: 1 mixing ammonium bicarbonate solution and antimony potassium tartrate solution.
3. The preparation method of the powder coating for the fire door as claimed in claim 2, wherein the powder coating comprises the following steps: the mass ratio of the sodium lignosulphonate to the silicon micro powder to the antimony potassium tartrate is 1-3:45-50: 6-10.
4. The preparation method of the powder coating for the fire door according to claim 1, wherein the powder coating comprises the following steps: the mass fraction of the benzoin in the ethanol dispersion liquid is 5-7%;
the mass fraction of ethanol is 40%.
5. The preparation method of the powder coating for the fire door according to claim 1, wherein the powder coating comprises the following steps: the weight parts of the calcined diatomite particles, the ethanol dispersion liquid and the cardanol are 14-16: 18-22: 0.5-0.9.
6. The preparation method of the powder coating for the fire door as claimed in claim 5, wherein the powder coating comprises the following steps: the preparation method of the calcined diatomite particles comprises the following steps:
adding diatomite into a resistance furnace, calcining for 1 hour at the temperature of 500-540 ℃, then naturally cooling to room temperature, grinding and sieving to obtain the diatomite powder;
the average particle size of the diatomaceous earth after sieving was 20 μm.
7. The preparation method of the powder coating for the fire door according to claim 1, wherein the powder coating comprises the following steps: the weight ratio of the composite silicon micropowder particles to the diatomite microparticles loaded with benzoin to the polyester resin powder to the curing agent to the leveling agent to the inorganic filler is (12-15: 4-5): 50-60: 4-5: 0.2-0.4:10-12.
8. The preparation method of the powder coating for the fire door according to claim 7, wherein the powder coating comprises the following steps: the weight part ratio of the composite silicon micropowder particles to the diatomite particles loaded with benzoin is 3: 1.
9. The method for preparing the powder coating for the fire door according to claim 1 or 7, wherein the method comprises the following steps: the curing agent is a beta-hydroxyalkylamide.
10. The method for preparing the powder coating for the fire door as claimed in claim 1 or 7, wherein the leveling agent is polydimethylsiloxane.
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