CN116102927B - Novel silver metallic paint coating material capable of transmitting millimeter radar waves and preparation method thereof - Google Patents
Novel silver metallic paint coating material capable of transmitting millimeter radar waves and preparation method thereof Download PDFInfo
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- CN116102927B CN116102927B CN202310208842.5A CN202310208842A CN116102927B CN 116102927 B CN116102927 B CN 116102927B CN 202310208842 A CN202310208842 A CN 202310208842A CN 116102927 B CN116102927 B CN 116102927B
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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
- C09D127/00—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 a halogen; Coating compositions based on derivatives of such polymers
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- C09D127/12—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/321—Phosphates
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Abstract
The invention relates to the technical field of millimeter-wave-transmitting radar wave materials, and particularly discloses a novel silver metallic paint coating material capable of transmitting millimeter radar waves, wherein the silver metallic paint coating material comprises the following raw materials in parts by weight: 60-70 parts of fluorocarbon resin, 15-20 parts of bidirectional coordination additive, 5-10 parts of silicone oil emulsion, 2-6 parts of flaky aluminum powder modifier, 3-6 parts of alcohol substance, 1-3 parts of aqueous defoamer, 1-2 parts of film forming agent, 2-5 parts of silane coupling agent KH560 and 55-65 parts of solvent. The invention improves the properties of the novel silver metallic paint coating material, such as millimeter-penetrating radar waves and adhesive force, and optimizes the coordination effect of the two properties by adding auxiliary agents such as alcohols and the like into the fluorocarbon resin, silicone oil emulsion, flaky aluminum powder modifier, bidirectional coordination additive and silane coupling agent KH 560.
Description
Technical Field
The invention relates to the technical field of millimeter-wave-transmitting radar wave materials, in particular to a novel silver metallic paint coating material capable of transmitting millimeter radar waves and a preparation method thereof.
Background
Currently, there are 24GHz,76.5GHz and 77GHz millimeter wave radars used in automobiles on a global scale. It is well known that metals have a shielding effect against electromagnetic waves. For paint with metallic silver effect, silver powder is generally selected as pigment, silver is a metallic material with excellent conductivity and has very high electromagnetic shielding effect, so that electromagnetic waves can be caused to have high attenuation phenomenon when penetrating, the silver paint used by millimeter wave radars used on automobiles at present meets the requirement of attenuation of different automobile grades, and the attenuation value of the automobile track grade is generally within 4dB and slightly different according to different automobile factories. However, silver is used as the main color of the automobile body, and is one of the main choices of automobile factories, and the front exterior trim part can be selected correspondingly. The process is used for meeting the requirements of radar wave transmission of the vehicle standard while the metallic paint is used. The silver metallic paint can meet the requirements of a vehicle factory from the color, but cannot meet the requirements of 4dB attenuation of a common vehicle gauge from the function, or the requirements of radar wave attenuation values cannot be met in the areas where radar waves specified by the vehicle factory penetrate through the exterior trim parts and part of the areas. The existing coating material has poor wave-transmitting performance, poor adhesive force with a base layer, low coordination performance of wave-transmitting and adhesive force, and reduced use efficiency of products, and based on the method, the invention further improves the product.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel silver metallic paint coating material capable of transmitting millimeter radar waves and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a novel silver metallic paint coating material capable of transmitting millimeter radar waves, which comprises the following raw materials in parts by weight:
60-70 parts of fluorocarbon resin, 15-20 parts of bidirectional coordination additive, 5-10 parts of silicone oil emulsion, 2-6 parts of flaky aluminum powder modifier, 3-6 parts of alcohol substance, 1-3 parts of aqueous defoamer, 1-2 parts of film forming agent, 2-5 parts of silane coupling agent KH560 and 55-65 parts of solvent.
Preferably, the silver metallic paint coating material comprises the following raw materials in parts by weight:
65 parts of fluorocarbon resin, 17.5 parts of bidirectional coordination additive, 7.5 parts of silicone oil emulsion, 4 parts of flaky aluminum powder modifier, 4.5 parts of alcohol substances, 2 parts of aqueous defoamer, 1.5 parts of film forming agent, 3.5 parts of silane coupling agent KH560 and 60 parts of solvent.
Preferably, the alcohol substance is one of 1, 6-hexanediol and neopentyl glycol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
Preferably, the preparation method of the bidirectional coordination additive comprises the following steps:
s11: placing graphene in 3-5 times of hydrochloric acid solution, stirring and dispersing uniformly, then adding sodium oxalate accounting for 1-5% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 5-10 parts of hydroxyapatite into 20-30 parts of ethanol, then adding 1-3 parts of glycolic acid and 0.2-0.5 part of silica sol, carrying out primary stirring reaction, adding 0.5-0.8 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding 10-15% of S12 product into the graphene complexing agent, stirring fully, washing with water, and drying to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 10-20% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1250-1550r/min, the ball milling time is 1-2h, and the bi-directional coordination additive is obtained after the ball milling is finished, washing and drying.
Preferably, the mass fraction of the hydrochloric acid solution is 3-6%.
Preferably, the rotation speed of the primary stirring reaction in the step S12 is 750-850r/min, the stirring time is 25-35min, and the stirring temperature is 40-43 ℃;
the rotation speed of the secondary stirring reaction is 150-250r/min, the stirring time is 55-65min, and the stirring temperature is 45-47 ℃.
Preferably, the modified ball grinding agent comprises the following raw materials in parts by weight:
2-5 parts of tannic acid, 15-20 parts of ethanol solvent, 1-4 parts of acetyl tributyl citrate, 0.3-0.4 part of gamma-aminopropyl trimethoxy silane and 0.1-0.3 part of yttrium nitrate.
Preferably, the preparation method of the flaky aluminum powder modifier comprises the following steps:
s11: adding (6-9) sheet aluminum powder into deionized water according to the weight ratio of 1, stirring uniformly, adding a phosphoric acid buffer solution accounting for 5-10% of the total amount of the sheet aluminum powder, and regulating the pH value, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5, so as to form a sheet aluminum powder dispersion liquid;
s12: then adding 5-10% of dimercaptopropane sodium sulfonate, 1-5% of chitosan water solution and 1-3% of lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain the flaky aluminum powder compound preparation.
Preferably, the particle size of the flaky aluminum powder is 5-15 microns, and the thickness is 0.2-0.5 microns; the mass fraction of the chitosan aqueous solution is 6-10%.
The invention also provides a preparation method of the novel silver metallic paint coating material capable of transmitting millimeter radar waves, which comprises the following steps:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material.
Compared with the prior art, the invention has the following beneficial effects:
according to the novel silver metallic paint coating material, through fluorocarbon resin, silicone oil emulsion, flaky aluminum powder modifier, bidirectional coordination additive and silane coupling agent KH560 raw materials, and through adding assistants such as alcohols, etc., the millimeter radar wave transmission performance and adhesive force performance of the product are improved, the performance coordination effect of the flaky aluminum powder modifier, the bidirectional coordination additive and the silane coupling agent KH560 is optimized, the interfacial properties of the flaky aluminum powder modifier and the bidirectional coordination additive are optimized, and the interfacial compatibility between the raw materials and organic raw materials such as fluorocarbon resin is improved; according to the bidirectional coordination additive, graphene is added to be treated by hydrochloric acid solution, sodium oxalate is added to form a graphene agent, so that the dispersibility and activity of the graphene are enhanced, the hydroxyapatite is subjected to primary reaction treatment by glycolic acid and silica sol, and then is subjected to secondary reaction treatment by diisooctyl phosphate, so that the modified hydroxyapatite is optimized in the graphene agent, can be better cooperated with graphene, the improvement of the effect of graphene on the penetrating millimeter radar wave and adhesive force performance in a product is improved, meanwhile, the modified graphene agent is subjected to ball milling modification by a modified ball mill, and the modified raw material is further coordinately improved on the adhesive force and the penetrating millimeter radar wave performance of the product in a system, so that the acid corrosion resistance performance of the product is enhanced, and the acid corrosion resistance stability of the product is improved; the added flaky aluminum powder modifier can be synergistic with the bidirectional coordination additive, so that the millimeter-penetrating radar wave and adhesive force coordination effect of the product is enhanced, and the performance efficiency of the product is further improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following raw materials in parts by weight:
60-70 parts of fluorocarbon resin, 15-20 parts of bidirectional coordination additive, 5-10 parts of silicone oil emulsion, 2-6 parts of flaky aluminum powder modifier, 3-6 parts of alcohol substance, 1-3 parts of aqueous defoamer, 1-2 parts of film forming agent, 2-5 parts of silane coupling agent KH560 and 55-65 parts of solvent.
The silver metallic paint coating material of the embodiment comprises the following raw materials in parts by weight:
65 parts of fluorocarbon resin, 17.5 parts of bidirectional coordination additive, 7.5 parts of silicone oil emulsion, 4 parts of flaky aluminum powder modifier, 4.5 parts of alcohol substances, 2 parts of aqueous defoamer, 1.5 parts of film forming agent, 3.5 parts of silane coupling agent KH560 and 60 parts of solvent.
The alcohol substance in the embodiment is one of 1, 6-hexanediol and neopentyl glycol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
The preparation method of the bidirectional coordination additive in the embodiment comprises the following steps:
s11: placing graphene in 3-5 times of hydrochloric acid solution, stirring and dispersing uniformly, then adding sodium oxalate accounting for 1-5% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 5-10 parts of hydroxyapatite into 20-30 parts of ethanol, then adding 1-3 parts of glycolic acid and 0.2-0.5 part of silica sol, carrying out primary stirring reaction, adding 0.5-0.8 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding 10-15% of S12 product into the graphene complexing agent, stirring fully, washing with water, and drying to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 10-20% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1250-1550r/min, the ball milling time is 1-2h, and the bi-directional coordination additive is obtained after the ball milling is finished, washing and drying.
The mass fraction of the hydrochloric acid solution of this example is 3-6%.
The rotational speed of the primary stirring reaction in the step S12 is 750-850r/min, the stirring time is 25-35min, and the stirring temperature is 40-43 ℃;
the rotation speed of the secondary stirring reaction is 150-250r/min, the stirring time is 55-65min, and the stirring temperature is 45-47 ℃.
The modified ball grinding agent comprises the following raw materials in parts by weight:
2-5 parts of tannic acid, 15-20 parts of ethanol solvent, 1-4 parts of acetyl tributyl citrate, 0.3-0.4 part of gamma-aminopropyl trimethoxy silane and 0.1-0.3 part of yttrium nitrate.
The preparation method of the flaky aluminum powder modifier in the embodiment comprises the following steps:
s11: adding (6-9) sheet aluminum powder into deionized water according to the weight ratio of 1, stirring uniformly, adding a phosphoric acid buffer solution accounting for 5-10% of the total amount of the sheet aluminum powder, and regulating the pH value, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5, so as to form a sheet aluminum powder dispersion liquid;
s12: then adding 5-10% of dimercaptopropane sodium sulfonate, 1-5% of chitosan water solution and 1-3% of lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain the flaky aluminum powder compound preparation.
The particle size of the flaky aluminum powder is 5-15 microns, and the thickness is 0.2-0.5 microns; the mass fraction of the chitosan aqueous solution is 6-10%.
The preparation method of the novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following steps:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material.
Example 1.
The novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following raw materials in parts by weight:
60 parts of fluorocarbon resin, 15 parts of bidirectional coordination additive, 5 parts of silicone oil emulsion, 2 parts of flaky aluminum powder modifier, 3 parts of alcohol substance, 1 part of aqueous defoamer, 1 part of film forming agent, 5602 parts of silane coupling agent KH and 55 parts of solvent.
The alcohol substance in the embodiment is 1, 6-hexanediol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
The preparation method of the bidirectional coordination additive in the embodiment comprises the following steps:
s11: placing graphene in a hydrochloric acid solution with the concentration of 3 times, stirring and dispersing uniformly, then adding sodium oxalate with the concentration of 1% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 5 parts of hydroxyapatite into 20 parts of ethanol, then adding 1 part of glycolic acid and 0.2 part of silica sol, carrying out primary stirring reaction, adding 0.5 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding 10% of S12 product into the graphene complexing agent, stirring fully, washing with water, and drying to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 10% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1250r/min, the ball milling time is 1h, and the two-way coordination additive is obtained after ball milling is finished, washing and drying.
The mass fraction of the hydrochloric acid solution of this example was 3%.
The rotation speed of the primary stirring reaction in the step S12 of the embodiment is 75r/min, the stirring time is 25min, and the stirring temperature is 40 ℃;
the rotating speed of the secondary stirring reaction is 150r/min, the stirring time is 55min, and the stirring temperature is 45 ℃.
The modified ball grinding agent comprises the following raw materials in parts by weight:
2 parts of tannic acid, 15 parts of ethanol solvent, 1 part of acetyl tributyl citrate, 0.3 part of gamma-aminopropyl trimethoxysilane and 0.1 part of yttrium nitrate.
The preparation method of the flaky aluminum powder modifier in the embodiment comprises the following steps:
s11: adding the flaky aluminum powder into deionized water according to the weight ratio of 1:6, uniformly stirring, adding a phosphoric acid buffer solution accounting for 5% of the total amount of the flaky aluminum powder, and adjusting the pH value, wherein the pH value of the phosphoric acid buffer solution is 4.5, so as to form a flaky aluminum powder dispersion;
s12: then adding 5% of dimercaptopropane sodium sulfonate, 1% of chitosan water solution and 1% of lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain the flaky aluminum powder compound preparation.
The particle size of the flaky aluminum powder in the embodiment is 5 microns, and the thickness is 0.2 microns; the mass fraction of the chitosan aqueous solution is 6%.
The preparation method of the novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following steps:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material.
Example 2.
The novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following raw materials in parts by weight:
70 parts of fluorocarbon resin, 20 parts of bidirectional coordination additive, 10 parts of silicone oil emulsion, 6 parts of flaky aluminum powder modifier, 6 parts of alcohol substance, 3 parts of aqueous defoamer, 2 parts of film forming agent, 5605 parts of silane coupling agent KH and 65 parts of solvent.
The alcohol in this example is neopentyl glycol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
The preparation method of the bidirectional coordination additive in the embodiment comprises the following steps:
s11: placing graphene in 5 times of hydrochloric acid solution, stirring and dispersing uniformly, then adding sodium oxalate accounting for 5% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 10 parts of hydroxyapatite into 30 parts of ethanol, then adding 3 parts of glycolic acid and 0.5 part of silica sol, carrying out primary stirring reaction, adding 0.8 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding 15% of S12 product into the graphene complexing agent, stirring fully, washing with water, and drying to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 20% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1550r/min, the ball milling time is 2h, and the two-way coordination additive is obtained after ball milling is finished, washing and drying.
The mass fraction of the hydrochloric acid solution of this example was 6%.
The rotational speed of the primary stirring reaction in S12 of the embodiment is 850r/min, the stirring time is 35min, and the stirring temperature is 43 ℃;
the rotating speed of the secondary stirring reaction is 250r/min, the stirring time is 65min, and the stirring temperature is 47 ℃.
The modified ball grinding agent comprises the following raw materials in parts by weight:
5 parts of tannic acid, 20 parts of ethanol solvent, 4 parts of acetyl tributyl citrate, 0.4 part of gamma-aminopropyl trimethoxysilane and 0.3 part of yttrium nitrate.
The preparation method of the flaky aluminum powder modifier in the embodiment comprises the following steps:
s11: adding the flaky aluminum powder into deionized water according to the weight ratio of 1:9, uniformly stirring, adding a phosphoric acid buffer solution accounting for 10% of the total amount of the flaky aluminum powder, and adjusting the pH value, wherein the pH value of the phosphoric acid buffer solution is 5.5, so as to form a flaky aluminum powder dispersion;
s12: then adding 10% of dimercaptopropane sodium sulfonate, 5% of chitosan water solution and 3% of lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain the flaky aluminum powder compound preparation.
The particle size of the flaky aluminum powder in the embodiment is 15 microns, and the thickness is 0.5 microns; the mass fraction of the chitosan aqueous solution is 10%.
The preparation method of the novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following steps:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material.
Example 3.
The novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following raw materials in parts by weight:
65 parts of fluorocarbon resin, 17.5 parts of bidirectional coordination additive, 7.5 parts of silicone oil emulsion, 4 parts of flaky aluminum powder modifier, 4.5 parts of alcohol substances, 2 parts of aqueous defoamer, 1.5 parts of film forming agent, 3.5 parts of silane coupling agent KH560 and 60 parts of solvent.
The alcohol in this example is neopentyl glycol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
The preparation method of the bidirectional coordination additive in the embodiment comprises the following steps:
s11: placing graphene in 4 times of hydrochloric acid solution, stirring and dispersing uniformly, then adding sodium oxalate accounting for 3% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 7.5 parts of hydroxyapatite into 25 parts of ethanol, then adding 2 parts of glycolic acid and 0.35 part of silica sol, carrying out primary stirring reaction, adding 0.65 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding an S12 product accounting for 12.5 percent of the total amount of the graphene complexing agent into the graphene complexing agent, stirring the mixture fully, and then washing and drying the mixture to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 15% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1400r/min, the ball milling time is 1.5h, and the two-way coordination additive is obtained after ball milling is finished, washing and drying.
The mass fraction of the hydrochloric acid solution of this example was 4.5%.
The rotation speed of the primary stirring reaction in the step S12 of the embodiment is 800r/min, the stirring time is 30min, and the stirring temperature is 42 ℃;
the rotation speed of the secondary stirring reaction is 200r/min, the stirring time is 60min, and the stirring temperature is 46 ℃.
The modified ball grinding agent comprises the following raw materials in parts by weight:
3.5 parts of tannic acid, 17 parts of ethanol solvent, 2.5 parts of acetyl tributyl citrate, 0.35 part of gamma-aminopropyl trimethoxysilane and 0.2 part of yttrium nitrate.
The preparation method of the flaky aluminum powder modifier in the embodiment comprises the following steps:
s11: adding the flaky aluminum powder into deionized water according to the weight ratio of 1:7.5, uniformly stirring, adding a phosphoric acid buffer solution accounting for 7.5% of the total amount of the flaky aluminum powder, and adjusting the pH value, wherein the pH value of the phosphoric acid buffer solution is 5.0, so as to form a flaky aluminum powder dispersion;
s12: then adding sodium dimercaptopropane sulfonate, 3% chitosan water solution and 2% lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain a flaky aluminum powder compound preparation; the particle size of the flaky aluminum powder is 10 microns, and the thickness of the flaky aluminum powder is 0.35 microns; the mass fraction of the chitosan aqueous solution is 8%.
The preparation method of the novel silver metallic paint coating material capable of transmitting millimeter radar waves comprises the following steps:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material.
Comparative example 1.
Unlike example 3, no bi-directional coordinating additive was added.
Comparative example 2.
The difference from example 3 is that the bi-directional co-ordination additive is replaced with graphene.
Comparative example 3.
The difference from example 3 is that the bi-directional co-ordinating additive is replaced by hydroxyapatite.
Comparative example 4.
The difference from example 3 is that the bi-directional coordination additive is replaced by mixing and stirring hydroxyapatite and graphene according to the weight ratio of 1:8.
Comparative example 5.
The difference from example 3 is that the graphene raw material in the preparation of the bi-directional co-ordination additive is replaced by nano silicon dioxide.
Comparative example 6.
The difference from example 3 is that the graphene complexing agent is replaced by graphene and deionized water according to the weight ratio of 1:4 in the preparation of the bidirectional coordination additive.
Comparative example 7.
The difference from example 3 is that the S12 product is replaced by a hydroxyapatite raw material in the preparation of the bi-directional co-ordinating additive.
Comparative example 8.
The difference from example 3 is that no silica sol was added in the preparation of the S12 product.
Comparative example 9.
The difference from example 3 is that no diisooctyl phosphate was added to the S12 product preparation.
Comparative example 10.
Unlike example 3, no glycolic acid was added in the preparation of the S12 product.
Comparative example 11.
The difference from example 3 is the process for the preparation of the S12 product:
adding 7.5 parts of hydroxyapatite into 25 parts of ethanol, then adding 2 parts of glycolic acid and 0.35 part of silica sol, then adding 0.65 part of diisooctyl phosphate, adopting the condition that the rotation speed is 800r/min, the stirring time is 60min and the stirring temperature is 46 ℃, and performing water washing and drying after the stirring is finished; namely, the high stirring rotation speed, the high stirring temperature and the high stirring time in the primary and secondary stirring are selected, and the primary and secondary stage fractional stirring treatment of the invention is not adopted except that the method is different.
Comparative example 12.
Different from the embodiment 3, the stirring conditions of the S12 are different, the rotation speed of the primary stirring reaction in the S12 is 200r/min, the stirring time is 30min, and the stirring temperature is 42 ℃; the rotation speed of the secondary stirring reaction is 800r/min, the stirring time is 60min, and the stirring temperature is 46 ℃.
Comparative example 13.
The difference from example 3 is that the modified ball mill is not added to the S14 ball milling treatment in the preparation of the bi-directional coordination additive.
Comparative example 14.
Unlike example 3, a modifier for flaky aluminum powder was not added.
Comparative example 15.
The difference from example 3 is that the modifier for flaky aluminum powder is replaced with flaky aluminum powder.
Comparative example 16.
Unlike example 3, lanthanum sulfate was not added in the preparation of the modifier for flaky aluminum powder.
Comparative example 17.
Unlike example 3, sodium dimercaptopropane sulfonate was not added in the preparation of the sheet aluminum powder modifier.
Comparative example 18.
The difference from example 3 is that no chitosan aqueous solution was added in the preparation of the modifier for flaky aluminum powder.
Comparative example 19.
The difference from example 3 is that the particle diameter of the flaky aluminum powder in the flaky aluminum powder modifier is 20 μm and the thickness is 0.6. Mu.m.
Comparative example 20.
The mass fraction of the aqueous chitosan solution in the modifier for flaky aluminum powder was 15% unlike example 3.
The paint is attached to the base material, PC is selected as the base material of the exterior trim part according to the requirements of a vehicle factory, the thickness of the base material is selected to be 4.5mm, the PC is baked for 2 hours at 120 ℃, the baking is finished, the cleaning is carried out, the surface energy is increased by flame treatment, the paint layer is sprayed, and the thickness is controlled to be 20 microns.
Under the test condition, the distance between the radar antenna and the product is 30mm, a 76.5GHz millimeter wave radar is adopted for bidirectional attenuation test, and the attenuation is tested by taking a test position with an azimuth angle of 10 degrees and an elevation angle of 30 degrees as an example; meanwhile, the adhesive force of the product and the performance effect between wave transmission are tested: and testing is divided into conventional conditions, and the product is simultaneously treated in 2% acid mist for 24 hours, and then tested for performance under the acid corrosion condition.
The results of the performance measurements of examples 1-3 and comparative examples 1-20 are as follows
The products of the embodiment 3 of the invention can reach the minimum attenuation of 0.31dB, the adhesive force can reach 15.9MPa, and the products have excellent acid corrosion stability under the acid corrosion condition;
as shown in comparative examples 1-4, no bidirectional coordination additive is added, the attenuation and adhesion of the product are obviously deteriorated, and the deterioration of the acid corrosion stability is more obvious; the bidirectional coordination additive is replaced by one of graphene and hydroxyapatite, the performance variation trend of the product is obvious, the bidirectional coordination additive is directly replaced by the ratio of the hydroxyapatite to the graphene, and the attenuation and adhesive force performance of the product are obvious;
the bidirectional coordination additive cannot be replaced by single raw materials of the bidirectional coordination additive, or the raw materials are directly assembled, and the bidirectional coordination additive is prepared by the method only, so that the performance effect is most remarkable;
according to the comparison example 5, the graphene raw materials are replaced by nano silicon dioxide in the preparation of the bidirectional coordination additive, the inventor discovers that the nano silicon dioxide and the hydroxyapatite are combined according to the optimized process, and the performance of the product is obviously worse under the acid corrosion condition than that of the product without the bidirectional coordination additive, so that the product is difficult to adapt to the acid corrosion condition by adopting the combination of the nano silicon dioxide and the hydroxyapatite, and meanwhile, the raw materials of the nano silicon dioxide and the hydroxyapatite are not combined by adopting the graphene and the hydroxyapatite under the conventional condition, so that the adhesive force and the wave transmission performance of the product are good, and in sum, only the method and the raw material selection are adopted, the prepared bidirectional coordination additive has the most remarkable improvement on the performance effect of the product, and other substitutions are not as good as the effect of the invention;
as can be seen from comparative examples 6 to 10, in the preparation of the bidirectional coordination additive, graphene and deionized water are adopted to replace the graphene complexing agent according to the weight ratio of 1:4, the performance of the product is poor, but the product S12 is not replaced by hydroxyapatite raw material, and the performance change of the product is obvious;
meanwhile, in the preparation of the S12 product, silica sol, diisooctyl phosphate and glycolic acid are not added, the performance of the product is prone to deterioration, diisooctyl phosphate is not added, and the performance of the product is most obviously changed; only adopting the process condition of S12, the prepared S12 product has the most obvious performance effect;
as shown in comparative examples 11-13, in the preparation of the S12 product, the preparation performance effects of the products under different stirring conditions are different, the products are not subjected to graded stirring, the performance of the products is prone to be degraded, and meanwhile, the fact that the S14 is not added with the modified ball milling agent for ball milling treatment is found that the performance change of the products is obvious under the acid corrosion condition, so that the treatment of the modified ball grinding agent has an important influence on the performance change of the products.
As shown in comparative examples 14-20, the product performance is obviously degraded without adding the flaky aluminum powder modifier, the flaky aluminum powder modifier can play a role in reinforcing the product, meanwhile, the flaky aluminum powder modifier is replaced by flaky aluminum powder, lanthanum sulfate, sodium dimercaptopropane sulfonate and chitosan aqueous solution are not added in the preparation of the flaky aluminum powder modifier, the product performance is in a degradation trend, and only the flaky aluminum powder modifier prepared by the method has the most obvious effects of adhesion, wave transmission performance coordination and acid corrosion stability, and the particle size, thickness and mass fraction of the chitosan aqueous solution of the flaky aluminum powder have influence on the product performance.
As shown in comparative example 1, comparative example 14 and example 3, the product performance deterioration is obvious without adding one of the flaky aluminum powder modifier and the bidirectional coordination additive, and the flaky aluminum powder modifier and the bidirectional coordination additive are matched, so that the product performance has a synergistic effect, the adhesive force of the product and the wave-transparent coordination effect are enhanced, and the stability effect of the product under the acid corrosion condition is improved.
The invention further explores the modified ball grinding agent:
the modified ball grinding agent comprises the following raw materials in parts by weight:
3.5 parts of tannic acid, 17 parts of ethanol solvent, 2.5 parts of acetyl tributyl citrate, 0.35 part of gamma-aminopropyl trimethoxysilane and 0.2 part of yttrium nitrate.
Experimental example 1
The same raw materials as those of the product of example 3 except that tannic acid was not added to the modified ball grinding agent.
Experimental example 2
The raw materials of the product are the same as those of the example 3, except that no acetyl tributyl citrate is added into the modified ball grinding agent.
Experimental example 3
The raw materials of the product are the same as those of the example 3, except that the gamma-aminopropyl trimethoxysilane is not added into the modified ball grinding agent.
Experimental example 4
The raw materials are the same as those of the product of example 3, except that yttrium nitrate is not added into the ball milling modification liquid.
The results of the product performance tests of examples 1-4 are as follows:
further research and demonstration are carried out on the modified ball grinding agent from experimental examples 1-4, the effect of adding no yttrium nitrate on the wave-transmitting and adhesive force performances of the product is the greatest under the conventional conditions, the effect of adding no tannic acid on the performances of the product is the greatest under the acid corrosion conditions, the effect of adding no gamma-aminopropyl trimethoxy silane on the performances of the product is the greatest, and the effect of adding acetyl tributyl citrate is the most remarkable by the mutual coordination among yttrium nitrate, tannic acid, gamma-aminopropyl trimethoxy silane and acetyl tributyl citrate, the adhesive force and the wave-transmitting coordination of the product are the most excellent under the conventional conditions, the acid corrosion stability is the most remarkable at the same time, and the proportioning effect of the modified ball grinding agent is not as remarkable by adopting other proportions.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. The novel silver metallic paint coating material capable of transmitting millimeter radar waves is characterized by comprising the following raw materials in parts by weight:
60-70 parts of fluorocarbon resin, 15-20 parts of bidirectional coordination additive, 5-10 parts of silicone oil emulsion, 2-6 parts of flaky aluminum powder modifier, 3-6 parts of alcohol substance, 1-3 parts of aqueous defoamer, 1-2 parts of film forming agent, 2-5 parts of silane coupling agent KH560 and 55-65 parts of solvent;
the preparation method of the bidirectional coordination additive comprises the following steps:
s11: placing graphene in 3-5 times of hydrochloric acid solution, stirring and dispersing uniformly, then adding sodium oxalate accounting for 1-5% of the total amount of the graphene, and stirring fully to obtain a graphene complexing agent;
s12: adding 5-10 parts of hydroxyapatite into 20-30 parts of ethanol, then adding 1-3 parts of glycolic acid and 0.2-0.5 part of silica sol, carrying out primary stirring reaction, adding 0.5-0.8 part of diisooctyl phosphate, continuing secondary stirring reaction, carrying out stirring reaction, washing with water, and drying;
s13: then adding 10-15% of S12 product into the graphene complexing agent, stirring fully, washing with water, and drying to obtain the hydroxyapatite modified graphene complexing agent;
s14: adding 10-20% of modified ball grinding agent into the hydroxyapatite modified graphene blending agent, then sending the mixture into a ball mill for ball milling reaction treatment, wherein the ball milling rotation speed of the ball milling reaction treatment is 1250-1550r/min, the ball milling time is 1-2h, and the two-way coordination additive is obtained after ball milling is finished, washing and drying; the preparation method of the flaky aluminum powder modifier comprises the following steps:
s11: adding (6-9) sheet aluminum powder into deionized water according to the weight ratio of 1, stirring uniformly, adding a phosphoric acid buffer solution accounting for 5-10% of the total amount of the sheet aluminum powder, and regulating the pH value, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5, so as to form a sheet aluminum powder dispersion liquid;
s12: then adding 5-10% of dimercaptopropane sodium sulfonate, 1-5% of chitosan water solution and 1-3% of lanthanum sulfate into the flaky aluminum powder dispersion, stirring thoroughly, washing with water and drying to obtain the flaky aluminum powder compound preparation.
2. The novel silver metallic paint coating material capable of transmitting millimeter radar waves according to claim 1, wherein the silver metallic paint coating material comprises the following raw materials in parts by weight:
65 parts of fluorocarbon resin, 17.5 parts of bidirectional coordination additive, 7.5 parts of silicone oil emulsion, 4 parts of flaky aluminum powder modifier, 4.5 parts of alcohol substances, 2 parts of aqueous defoamer, 1.5 parts of film forming agent, 3.5 parts of silane coupling agent KH560 and 60 parts of solvent.
3. The novel silver metallic paint coating material capable of transmitting millimeter radar waves according to claim 1, wherein the alcohol substance is one of 1, 6-hexanediol and neopentyl glycol; the solvent is cyclohexanone; the water-based defoamer is 901W in Digao; the film forming agent is propylene glycol diethyl ether.
4. A novel silver metallic paint coating material permeable to millimeter radar waves as recited in claim 1, wherein the mass fraction of the hydrochloric acid solution is 3-6%.
5. The novel silver metallic paint coating material capable of penetrating millimeter radar waves, according to claim 1, wherein the rotation speed of the primary stirring reaction in the step S12 is 750-850r/min, the stirring time is 25-35min, and the stirring temperature is 40-43 ℃;
the rotation speed of the secondary stirring reaction is 150-250r/min, the stirring time is 55-65min, and the stirring temperature is 45-47 ℃.
6. The novel silver metallic paint coating material capable of transmitting millimeter radar waves as claimed in claim 1, wherein the modified ball grinding agent comprises the following raw materials in parts by weight:
2-5 parts of tannic acid, 15-20 parts of ethanol solvent, 1-4 parts of acetyl tributyl citrate, 0.3-0.4 part of gamma-aminopropyl trimethoxy silane and 0.1-0.3 part of yttrium nitrate.
7. The novel silver metallic paint coating material capable of transmitting millimeter radar waves according to claim 1, wherein the particle size of the flaky aluminum powder is 5-15 microns and the thickness is 0.2-0.5 microns; the mass fraction of the chitosan aqueous solution is 6-10%.
8. A method for preparing a novel metallic silver paint coating material permeable to millimeter radar waves as claimed in any one of claims 1 to 7, comprising the steps of:
step one: weighing the raw materials:
step two: feeding the flaky aluminum powder modifier, the bidirectional coordination additive, the silane coupling agent KH560 and the solvent into a stirrer for stirring until the raw materials are uniformly mixed;
step three: and sequentially adding fluorocarbon resin, silicone oil emulsion, alcohol substances, water-based defoamer and film forming agent into the stirrer in the second step, continuously and fully stirring, and obtaining the silver metallic paint coating material after stirring.
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| CN103224228A (en) * | 2013-04-07 | 2013-07-31 | 怀化学院 | Selectively reduced graphene oxide and preparation method |
| CN114075390A (en) * | 2020-08-20 | 2022-02-22 | 海洋化工研究院有限公司 | High seaworthiness heat reflection wave-transparent coating, preparation method and application |
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| CN102127361A (en) * | 2011-01-31 | 2011-07-20 | 中国人民解放军91872部队 | Light-color antistatic coating with high electromagnetic wave transmissivity and preparation method thereof |
| CN103224228A (en) * | 2013-04-07 | 2013-07-31 | 怀化学院 | Selectively reduced graphene oxide and preparation method |
| CN114075390A (en) * | 2020-08-20 | 2022-02-22 | 海洋化工研究院有限公司 | High seaworthiness heat reflection wave-transparent coating, preparation method and application |
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