CN112920628A - Vehicle paint maintenance coating agent and preparation method thereof - Google Patents
Vehicle paint maintenance coating agent and preparation method thereof Download PDFInfo
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- CN112920628A CN112920628A CN202110107463.8A CN202110107463A CN112920628A CN 112920628 A CN112920628 A CN 112920628A CN 202110107463 A CN202110107463 A CN 202110107463A CN 112920628 A CN112920628 A CN 112920628A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D403/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00
- C07D403/14—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing three or more hetero rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D417/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00
- C07D417/14—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00 containing three or more hetero rings
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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
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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Abstract
The invention discloses a car paint maintenance coating agent and a preparation method thereof, wherein the coating agent comprises the following raw materials by weight: 5-10 parts of ethyl orthosilicate, 5-10 parts of ethyl orthotitanate, 5-8 parts of ethanol, 20-30 parts of deionized water, 3-5 parts of an oxidation resistant agent and 1-3 parts of a film forming auxiliary agent; the anti-oxidant is prepared in the process of preparing the coating agent, the molecular weight of the anti-oxidant is high, so that after the coating agent is formed into a film, oxidation-resistant components cannot be separated out from the interior of the paint film in the process of long-time use, the protection time of the coating agent on the paint film is longer, the anti-oxidant contains a large amount of hindered phenol and sulfur atoms, the sulfur atoms are easily oxidized into sulfoxide and brazil compounds, a hydrogen bond chelating ring exists in the molecule of the anti-oxidant, after ultraviolet rays are absorbed, the hydrogen bond is destroyed, ultraviolet light energy is converted into heat energy to be released, the coating agent is enabled not to be easily oxidized after the coating agent forms a glass film, the integrity of the glass film is further ensured, and the paint.
Description
Technical Field
The invention relates to the technical field of vehicle paint maintenance, in particular to a vehicle paint maintenance coating agent and a preparation method thereof.
Background
Automobiles are one of the modern vehicles, and the use of automobiles is increasingly common. The automobile shell is usually made of thin steel plates, a layer of paint is sprayed on the surface of the automobile shell, and because the automobile is driven and parked outside for a long time, and is exposed to the sun and rain, and dust pollution caused by wind and dust is inevitable, a protective layer is coated on the automobile shell to prevent the automobile shell from being corroded by external harmful substances, and the paint layer is required to be bright and attractive. At present, automobile surface glazing protection products widely used at home and abroad are mainly automobile glazing wax, the main functions of the automobile glazing wax are glazing and nursing automobile paint surfaces, a layer of protection film is formed on the automobile surface, the protection film is waterproof and dustproof, the glossiness is improved, and the appearance of a film coating agent gradually transfers the eyesight to the film coating agent.
The pencil hardness of the existing car paint maintenance coating agent can reach 7H, but in the using process, the coating agent is influenced by oxygen, ultraviolet rays and high temperature in the air to generate an aging phenomenon, so that the pencil hardness of the coating agent is reduced, and the car paint protection effect cannot be achieved.
Disclosure of Invention
The invention aims to provide a car paint maintenance coating agent and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the pencil hardness of the existing car paint maintenance coating agent can reach 7H, but in the using process, the coating agent is influenced by oxygen, ultraviolet rays and high temperature in the air to generate an aging phenomenon, so that the pencil hardness of the coating agent is reduced, and the car paint protection effect cannot be achieved.
The purpose of the invention can be realized by the following technical scheme:
the vehicle paint maintenance coating agent comprises the following raw materials in parts by weight: 5-10 parts of ethyl orthosilicate, 5-10 parts of ethyl orthotitanate, 5-8 parts of ethanol, 20-30 parts of deionized water, 3-5 parts of an oxidation resistant agent and 1-3 parts of a film forming auxiliary agent;
the vehicle paint maintenance coating agent is prepared by the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h under the conditions that the rotating speed is 200-300r/min and the temperature is 70-80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h at the rotation speed of 200-300r/min and the temperature of 80-85 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1-1.5h under the condition that the rotating speed is 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 2-3h to prepare the car paint maintenance coating agent.
Further, the film-forming assistant is one or a mixture of more of dodecyl alcohol ester, hexanediol and ethylene glycol in any proportion.
Further, the oxidation resistant agent is prepared by the following steps:
step A1: adding deionized water and concentrated hydrochloric acid into a reaction kettle, stirring and adding o-nitroaniline under the condition that the rotation speed is 500-800r/min, stirring at the temperature of 60-70 ℃, cooling to the temperature of 1-3 ℃ after the o-nitroaniline is completely dissolved, adding sodium nitrite, reacting for 3-5h to obtain a diazo solution, adding sodium carbonate, m-aminophenol and the diazo solution into the reaction kettle, stirring at the rotation speed of 200-300r/min and the temperature of 1-3 ℃ for 10-15min, adjusting the pH value of the mixed solution to 9-10, and continuing to react for 2-3h to obtain an intermediate 1;
the reaction process is as follows:
step A2: adding deionized water and sodium hydroxide into a reaction kettle, stirring and adding the intermediate 1 prepared in the step A2 under the condition that the rotating speed is 600-800r/min, adding thiourea dioxide at the temperature of 70-75 ℃ for 20-30min, and reacting at the temperature of 80-90 ℃ for 3-5h after the addition is finished to prepare an intermediate 2;
the reaction process is as follows:
step A3: dissolving cyanuric chloride in ether, adding aluminum trichloride and 5-methyl salicylic acid under the conditions of the rotation speed of 200-90 ℃ and the temperature of 80-90 ℃ for reaction for 4-6h to prepare an intermediate 3, adding the intermediate 3, the intermediate 2 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole under the conditions of the rotation speed of 150-200r/min and the temperature of 25-30 ℃ for reaction for 5-8h to prepare an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, reacting at the temperature of 85-90 ℃ for 3-5h to prepare an intermediate 5, adding the intermediate 5, deionized water and potassium permanganate into the reaction kettle, performing reflux reaction at the temperature of 110-120 ℃ for 4-5h, to prepare an intermediate 6;
the reaction process is as follows:
step A4: adding o-nitrophenol, formaldehyde and ethanol into a reaction kettle, adding dimethylamine aqueous solution at the temperature of 30-35 ℃, reflux reaction is carried out for 3-5h at the temperature of 80-85 ℃ to prepare an intermediate 7, the intermediate 7, p-methyl benzene methyl mercaptan and N, N-dimethylformamide are added into a reaction kettle, nitrogen is introduced for protection, carrying out reflux reaction for 7-9h at the rotation speed of 150-200r/min and the temperature of 120-130 ℃ to obtain an intermediate 8, adding the intermediate 8, iron powder and ethanol into a reaction kettle, carrying out reflux reaction for 3-5h at the temperature of 80-85 ℃, adding a hydrochloric acid solution for 20-30min, continuously reacting for 5-6h, and adjusting the pH value of the reaction solution to 7 to prepare an intermediate 9;
the reaction process is as follows:
step A5: dissolving an intermediate 9 in tetrahydrofuran, introducing chlorine, reacting for 1-2h under the condition of illumination to obtain an intermediate 10, adding the intermediate 10, an intermediate 6 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxybenzotriazole under the conditions of a rotation speed of 150-, dissolving the intermediate 13 in tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished, filtering to remove filtrate, and distilling the filtrate to remove tetrahydrofuran to obtain the antioxidant.
The reaction process is as follows:
further, the using amount ratio of the deionized water, the concentrated hydrochloric acid, the o-nitroaniline and the sodium nitrite in the step A1 is 5mL:5.3mL:2g:1g, the mass fraction of the concentrated hydrochloric acid is 36%, and the using amount ratio of the sodium carbonate, the m-aminophenol and the diazo solution is 2.3g:1.2g:6 mL.
Furthermore, the using ratio of the deionized water, the sodium hydroxide, the intermediate 1 and the thiourea dioxide in the step A2 is 150mL:8g:6.5g:10 g.
Further, the molar ratio of the cyanuric chloride to the 5-methyl salicylic acid in the step A3 is 1:3, the molar ratio of the aluminum trichloride is 10-15% of the mass of the 5-methyl salicylic acid, the molar ratio of the intermediate 3 to the intermediate 2 is 1:3, the amount of 1-hydroxy benzotriazole is 35% of the mass of the intermediate 3, the amount of the intermediate 4, potassium carbonate and dimethyl sulfate is 3:1:4, and the amount ratio of the intermediate 5, deionized water and potassium permanganate is 2g:80 mL:5.
Further, in the step A4, the dosage ratio of the o-nitrophenol, the formaldehyde, the ethanol and the dimethylamine is 1mol:3mol:50mL:3mol, the dosage ratio of the intermediate 7, the p-methyl benzenethiol and the N, N-dimethylformamide is 0.5mol:1mol:100mL, the dosage ratio of the intermediate 8, the iron powder, the ethanol and the hydrochloric acid solution is 2g:4.5g:60mL:10mL, the volume fraction of the ethanol is 90%, the hydrochloric acid solution is concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% are mixed according to the volume ratio of 1: 9.
Further, the molar ratio of the amount of the intermediate 9 to the chlorine in the step A5 is 1:3, the molar ratio of the amount of the intermediate 10 to the amount of the intermediate 6 is 1:1, the amount of 1-hydroxybenzotriazole is 20-25% of the amount of the intermediate 10, the amount of diphenylamine, sulfur and iodine is 21.5:8:0.15, the molar ratio of the amount of the intermediate 11 to the amount of the intermediate 12 is 1:6, and the amount of the intermediate 7 to the amount of boron tribromide is 1g:5 mL.
A preparation method of a car paint maintenance coating agent specifically comprises the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h under the conditions that the rotating speed is 200-300r/min and the temperature is 70-80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h at the rotation speed of 200-300r/min and the temperature of 80-85 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1-1.5h under the condition that the rotating speed is 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 2-3h to prepare the car paint maintenance coating agent.
The invention has the beneficial effects that: the invention prepares an oxidation-resistant agent in the process of preparing a car paint maintenance coating agent, the oxidation-resistant agent takes o-nitroaniline as raw material to prepare diazo solution, the diazo solution reacts with m-aminophenol to prepare an intermediate 1, the intermediate 1 is further processed to prepare an intermediate 2, cyanuric chloride and 5-methyl salicylic acid react under the action of aluminum trichloride to prepare an intermediate 3, the intermediate 3 and the intermediate 2 are condensed under the action of 1-hydroxybenzotriazole, carboxyl on the intermediate 3 and amino on the intermediate 2 to prepare an intermediate 4, the intermediate 4 is subjected to hydroxyl protection to prepare an intermediate 5, the intermediate 5 is oxidized to oxidize methyl on a benzene ring to form carboxyl to prepare an intermediate 6, the o-nitrophenol, formaldehyde and dimethylamine react to prepare an intermediate 7, the intermediate 7 reacts with methyl benzyl mercaptan, preparing an intermediate 8, reducing the intermediate 8 to convert nitro into amino to prepare an intermediate 9, replacing a reaction intermediate 10 by the intermediate 9 and chlorine under the illumination condition, condensing the intermediate 6 and the intermediate 10 under the action of 1-hydroxybenzotriazole to prepare an intermediate 11, reacting diphenylamine and sulfur to prepare an intermediate 12, reacting the intermediate 11 and the intermediate 12 to prepare an intermediate 13, deprotecting the intermediate 13 to prepare an oxidation-resistant agent, wherein the oxidation-resistant agent has high molecular weight, so that oxidation-resistant components cannot be separated out from the inside of a paint film in the long-term use process after a film coating agent is formed, the paint film is protected by the coating agent for a longer time, the coating agent contains a large amount of hindered phenol and sulfur atoms, the sulfur atoms are easily oxidized into sulfoxide and sulfoxide compounds, and the oxidation-resistant agent has a hydrogen bond chelating ring in the molecule, after absorbing ultraviolet rays, the hydrogen bonds are destroyed, and ultraviolet light energy is converted into heat energy to be released, so that the film coating agent is not easy to be oxidized after forming a glass film, the integrity of the glass film is further ensured, and the paint film is protected from being damaged.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The vehicle paint maintenance coating agent comprises the following raw materials in parts by weight: 5 parts of ethyl orthosilicate, 5 parts of ethyl orthotitanate, 5 parts of ethanol, 20 parts of deionized water, 3 parts of an oxidation resistant agent and 1 part of a film-forming assistant;
the vehicle paint maintenance coating agent is prepared by the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3 hours at the rotating speed of 200r/min and the temperature of 70 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half of ethanol and half of deionized water into a reaction kettle, and stirring for 3 hours at the rotating speed of 200r/min and the temperature of 80 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1 hour at the rotating speed of 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 2 hours to prepare the car paint maintenance coating agent.
The oxidation resistant agent is prepared by the following steps:
step A1: adding deionized water and concentrated hydrochloric acid into a reaction kettle, stirring and adding o-nitroaniline under the condition that the rotation speed is 500r/min, stirring at the temperature of 60 ℃ until the o-nitroaniline is completely dissolved, cooling to the temperature of 1 ℃, adding sodium nitrite, reacting for 3 hours to obtain a diazo solution, adding sodium carbonate, m-aminophenol and the diazo solution into the reaction kettle, stirring at the rotation speed of 200r/min and the temperature of 1 ℃ for 10 minutes, adjusting the pH value of the mixed solution to 9, and continuing to react for 2 hours to obtain an intermediate 1;
step A2: adding deionized water and sodium hydroxide into a reaction kettle, stirring and adding the intermediate 1 prepared in the step A2 under the condition that the rotating speed is 600r/min, adding thiourea dioxide at the temperature of 70 ℃, adding for 20min, and reacting for 3h under the condition that the temperature is 80 ℃ after the addition is finished to prepare an intermediate 2;
step A3: dissolving cyanuric chloride in diethyl ether, adding sodium acetate and 5-methyl salicylic acid at the conditions of the rotation speed of 200r/min and the temperature of 80 ℃ for reaction for 4h to prepare an intermediate 3, adding the intermediate 3, the intermediate 2 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole at the conditions of the rotation speed of 150r/min and the temperature of 25 ℃ for reaction for 5h to prepare an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, reacting for 3h at the temperature of 85 ℃ to prepare an intermediate 5, adding the intermediate 5, deionized water and potassium permanganate into the reaction kettle, and performing reflux reaction for 4h at the temperature of 110 ℃ to prepare an intermediate 6;
step A4: adding o-nitrophenol, formaldehyde and ethanol into a reaction kettle, adding dimethylamine aqueous solution at the temperature of 30 ℃, performing reflux reaction for 3 hours at the temperature of 80 ℃ to obtain an intermediate 7, adding the intermediate 7, p-methyl benzenethiol and N, N-dimethylformamide into the reaction kettle, introducing nitrogen for protection, performing reflux reaction for 7 hours at the rotation speed of 150r/min and the temperature of 120 ℃ to obtain an intermediate 8, adding the intermediate 8, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3 hours at the temperature of 80 ℃, adding hydrochloric acid solution, adding the hydrochloric acid solution for 20 minutes, continuously reacting for 5 hours, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 9;
step A5: adding the intermediate 9, the intermediate 6 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxybenzotriazole under the conditions of the rotating speed of 150r/min and the temperature of 25 ℃, reacting for 5 hours to obtain an intermediate 10, dissolving the intermediate 10 in tetrahydrofuran, introducing chlorine, reacting for 1 hour under the condition of illumination to obtain an intermediate 11, adding diphenylamine, sulfur and iodine into the reaction kettle, introducing nitrogen for protection, stirring under the conditions of the rotating speed of 120r/min and the temperature of 180 ℃ to obtain an intermediate 12, adding the intermediate 11, the intermediate 12 and ethanol into the reaction kettle, performing reflux reaction for 4 hours under the conditions of the rotating speed of 200r/min and the temperature of 80 ℃ to obtain an intermediate 13, dissolving the intermediate 13 in tetrahydrofuran, adding boron tribromide at the temperature of 70 ℃ below zero, adding after the addition is finished, reacting at 25 deg.C for 10 hr, filtering to remove filtrate, and distilling the filtrate to remove tetrahydrofuran to obtain the antioxidant.
Example 2
The vehicle paint maintenance coating agent comprises the following raw materials in parts by weight: 8 parts of ethyl orthosilicate, 8 parts of ethyl orthotitanate, 6 parts of ethanol, 25 parts of deionized water, 4 parts of an oxidation resistant agent and 2 parts of a film-forming assistant;
the vehicle paint maintenance coating agent is prepared by the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3 hours at the rotating speed of 200r/min and the temperature of 80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half of ethanol and half of deionized water into a reaction kettle, and stirring for 5 hours at the rotating speed of 300r/min and the temperature of 80 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1 hour at the rotating speed of 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 3 hours to prepare the car paint maintenance coating agent.
The oxidation resistant agent is prepared by the following steps:
step A1: adding deionized water and concentrated hydrochloric acid into a reaction kettle, stirring and adding o-nitroaniline under the condition that the rotation speed is 500r/min, stirring at the temperature of 70 ℃ until the o-nitroaniline is completely dissolved, cooling to the temperature of 1 ℃, adding sodium nitrite, reacting for 5 hours to obtain a diazo solution, adding sodium carbonate, m-aminophenol and the diazo solution into the reaction kettle, stirring at the rotation speed of 200r/min and the temperature of 3 ℃ for 10 minutes, adjusting the pH value of the mixed solution to 10, and continuing to react for 2 hours to obtain an intermediate 1;
step A2: adding deionized water and sodium hydroxide into a reaction kettle, stirring and adding the intermediate 1 prepared in the step A2 under the condition that the rotating speed is 800r/min, adding thiourea dioxide at the temperature of 70 ℃, adding for 30min, and reacting for 5h at the temperature of 80 ℃ after the addition is finished to prepare an intermediate 2;
step A3: dissolving cyanuric chloride in diethyl ether, adding sodium acetate and 5-methyl salicylic acid at the rotation speed of 200r/min and the temperature of 90 ℃ for reaction for 4h to obtain an intermediate 3, adding the intermediate 3, the intermediate 2 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole at the rotation speed of 200r/min and the temperature of 25 ℃ for reaction for 8h to obtain an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, reacting for 5h at the temperature of 85 ℃ to obtain an intermediate 5, adding the intermediate 5, deionized water and potassium permanganate into the reaction kettle, and performing reflux reaction for 5h at the temperature of 110 ℃ to obtain an intermediate 6;
step A4: adding o-nitrophenol, formaldehyde and ethanol into a reaction kettle, adding dimethylamine aqueous solution at the temperature of 30 ℃, performing reflux reaction for 3 hours at the temperature of 85 ℃ to obtain an intermediate 7, adding the intermediate 7, p-methyl benzenethiol and N, N-dimethylformamide into the reaction kettle, introducing nitrogen for protection, performing reflux reaction for 9 hours at the rotation speed of 200r/min and the temperature of 120 ℃ to obtain an intermediate 8, adding the intermediate 8, iron powder and ethanol into the reaction kettle, performing reflux reaction for 5 hours at the temperature of 80 ℃, adding hydrochloric acid solution, adding the hydrochloric acid solution for 20 minutes, continuously reacting for 6 hours, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 9;
step A5: adding the intermediate 9, the intermediate 6 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole into the reaction kettle at the rotation speed of 150r/min and the temperature of 30 ℃ for reaction for 5 hours to obtain an intermediate 10, dissolving the intermediate 10 in tetrahydrofuran, introducing chlorine gas, reacting for 2 hours under the illumination condition to obtain an intermediate 11, adding diphenylamine, sulfur and iodine into the reaction kettle, introducing nitrogen gas for protection, stirring at the rotation speed of 120r/min and the temperature of 190 ℃ to obtain an intermediate 12, adding the intermediate 11, the intermediate 12 and ethanol into the reaction kettle, performing reflux reaction for 4 hours at the rotation speed of 200r/min and the temperature of 85 ℃ to obtain an intermediate 13, dissolving the intermediate 13 in tetrahydrofuran, adding boron tribromide at the temperature of 80 ℃ below zero, and after the addition is finished, reacting at 25 deg.C for 15 hr, filtering to remove filtrate, and distilling the filtrate to remove tetrahydrofuran to obtain the antioxidant.
Example 3
The vehicle paint maintenance coating agent comprises the following raw materials in parts by weight: 10 parts of ethyl orthosilicate, 10 parts of ethyl orthotitanate, 8 parts of ethanol, 30 parts of deionized water, 5 parts of an oxidation resistant agent and 3 parts of a film forming auxiliary agent;
the vehicle paint maintenance coating agent is prepared by the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 5 hours at the rotating speed of 300r/min and the temperature of 80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half of ethanol and half of deionized water into a reaction kettle, and stirring for 5 hours at the rotating speed of 300r/min and the temperature of 85 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1.5 hours at the rotating speed of 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 3 hours to prepare the car paint maintenance coating agent.
The oxidation resistant agent is prepared by the following steps:
step A1: adding deionized water and concentrated hydrochloric acid into a reaction kettle, stirring and adding o-nitroaniline under the condition that the rotation speed is 800r/min, stirring at the temperature of 70 ℃ until the o-nitroaniline is completely dissolved, cooling to the temperature of 3 ℃, adding sodium nitrite, reacting for 5 hours to obtain a diazo solution, adding sodium carbonate, m-aminophenol and the diazo solution into the reaction kettle, stirring at the rotation speed of 300r/min and the temperature of 3 ℃ for 15 minutes, adjusting the pH value of the mixed solution to 10, and continuing to react for 3 hours to obtain an intermediate 1;
step A2: adding deionized water and sodium hydroxide into a reaction kettle, stirring and adding the intermediate 1 prepared in the step A2 under the condition that the rotating speed is 800r/min, adding thiourea dioxide at the temperature of 75 ℃ for 30min, and reacting for 5h at the temperature of 90 ℃ after the addition is finished to prepare an intermediate 2;
step A3: dissolving cyanuric chloride in diethyl ether, adding sodium acetate and 5-methyl salicylic acid at the rotation speed of 300r/min and the temperature of 90 ℃ for reaction for 6h to obtain an intermediate 3, adding the intermediate 3, the intermediate 2 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole at the rotation speed of 200r/min and the temperature of 30 ℃ for reaction for 8h to obtain an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, reacting for 5h at the temperature of 90 ℃ to obtain an intermediate 5, adding the intermediate 5, deionized water and potassium permanganate into the reaction kettle, and performing reflux reaction for 5h at the temperature of 120 ℃ to obtain an intermediate 6;
step A4: adding o-nitrophenol, formaldehyde and ethanol into a reaction kettle, adding dimethylamine aqueous solution at the temperature of 35 ℃, performing reflux reaction for 5 hours at the temperature of 85 ℃ to obtain an intermediate 7, adding the intermediate 7, p-methyl benzenethiol and N, N-dimethylformamide into the reaction kettle, introducing nitrogen for protection, performing reflux reaction for 9 hours at the rotation speed of 200r/min and the temperature of 130 ℃ to obtain an intermediate 8, adding the intermediate 8, iron powder and ethanol into the reaction kettle, performing reflux reaction for 5 hours at the temperature of 85 ℃, adding hydrochloric acid solution, adding the hydrochloric acid solution for 30 minutes, continuously reacting for 6 hours, and adjusting the pH value of the reaction solution to 7 to obtain an intermediate 9;
step A5: adding the intermediate 9, the intermediate 6 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole into the reaction kettle at the rotation speed of 200r/min and the temperature of 30 ℃ for reaction for 8 hours to obtain an intermediate 10, dissolving the intermediate 10 in tetrahydrofuran, introducing chlorine gas, reacting for 2 hours under the illumination condition to obtain an intermediate 11, adding diphenylamine, sulfur and iodine into the reaction kettle, introducing nitrogen gas for protection, stirring at the rotation speed of 150r/min and the temperature of 190 ℃ to obtain an intermediate 12, adding the intermediate 11, the intermediate 12 and ethanol into the reaction kettle, performing reflux reaction for 6 hours under the rotation speed of 300r/min and the temperature of 85 ℃ to obtain an intermediate 13, dissolving the intermediate 13 in tetrahydrofuran, adding boron tribromide at the temperature of 80 ℃ below zero, and after the addition is finished, reacting at 30 deg.C for 15 hr, filtering to remove filtrate, and distilling the filtrate to remove tetrahydrofuran to obtain the antioxidant.
Comparative example
The comparative example is a common car paint maintenance coating agent in the market.
The coating agents prepared in examples 1 to 3 and comparative example were subjected to performance tests, and the test results are shown in table 1 below;
coating the coating agents prepared in examples 1 to 3 and comparative example on a flat plate, detecting the pencil hardness of the coating after the coating is completely solidified, placing the flat plate at the indoor temperature of 30 ℃ for 30 days, detecting the pencil hardness of the coating, taking the newly formed flat plate, and irradiating with the light with the wavelength of 340nm and the irradiation intensity of 0.68W/m2The temperature of the blackboard is 60 ℃, and the condensation temperature is 60 ℃; a single cycle process; illuminating for 3h, and blowing for 10 min; continuously repeating the cycle process, wherein the total experiment time is 168h, and the pencil hardness is detected;
TABLE 1
As can be seen from Table 1 above, the coating agents prepared in examples 1 to 3 were allowed to stand at 30 ℃ for 30 days and had pencil hardness of 7H, and after aging test, had pencil hardness of 7H, which was the same as that of the pencil under normal conditions, while the coating agent prepared in comparative example had pencil hardness of 6H, and after aging test, had pencil hardness of 5H, which was decreased from that of the pencil under normal conditions, after standing at 30 ℃ for 30 days.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (9)
1. The car paint maintenance coating agent is characterized in that: comprises the following raw materials by weight: 5-10 parts of ethyl orthosilicate, 5-10 parts of ethyl orthotitanate, 5-8 parts of ethanol, 20-30 parts of deionized water, 3-5 parts of an oxidation resistant agent and 1-3 parts of a film forming auxiliary agent;
the vehicle paint maintenance coating agent is prepared by the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h under the conditions that the rotating speed is 200-300r/min and the temperature is 70-80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h at the rotation speed of 200-300r/min and the temperature of 80-85 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1-1.5h under the condition that the rotating speed is 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 2-3h to prepare the car paint maintenance coating agent.
2. The vehicle paint maintenance coating agent of claim 1, wherein: the film-forming assistant is one or a mixture of more of dodecyl alcohol ester, hexanediol and ethylene glycol in any proportion.
3. The vehicle paint maintenance coating agent of claim 1, wherein: the oxidation resistant agent is prepared by the following steps:
step A1: adding deionized water and concentrated hydrochloric acid into a reaction kettle, stirring and adding o-nitroaniline under the condition that the rotation speed is 500-800r/min, stirring at the temperature of 60-70 ℃, cooling to the temperature of 1-3 ℃ after the o-nitroaniline is completely dissolved, adding sodium nitrite, reacting for 3-5h to obtain a diazo solution, adding sodium carbonate, m-aminophenol and the diazo solution into the reaction kettle, stirring at the rotation speed of 200-300r/min and the temperature of 1-3 ℃ for 10-15min, adjusting the pH value of the mixed solution to 9-10, and continuing to react for 2-3h to obtain an intermediate 1;
step A2: adding deionized water and sodium hydroxide into a reaction kettle, stirring and adding the intermediate 1 prepared in the step A2 under the condition that the rotating speed is 600-800r/min, adding thiourea dioxide at the temperature of 70-75 ℃ for 20-30min, and reacting at the temperature of 80-90 ℃ for 3-5h after the addition is finished to prepare an intermediate 2;
step A3: dissolving cyanuric chloride in ether, adding aluminum trichloride and 5-methyl salicylic acid under the conditions of the rotation speed of 200-90 ℃ and the temperature of 80-90 ℃ for reaction for 4-6h to prepare an intermediate 3, adding the intermediate 3, the intermediate 2 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxy benzotriazole under the conditions of the rotation speed of 150-200r/min and the temperature of 25-30 ℃ for reaction for 5-8h to prepare an intermediate 4, adding the intermediate 4, potassium carbonate, dimethyl sulfate and acetone into the reaction kettle, reacting at the temperature of 85-90 ℃ for 3-5h to prepare an intermediate 5, adding the intermediate 5, deionized water and potassium permanganate into the reaction kettle, performing reflux reaction at the temperature of 110-120 ℃ for 4-5h, to prepare an intermediate 6;
step A4: adding o-nitrophenol, formaldehyde and ethanol into a reaction kettle, adding dimethylamine aqueous solution at the temperature of 30-35 ℃, reflux reaction is carried out for 3-5h at the temperature of 80-85 ℃ to prepare an intermediate 7, the intermediate 7, p-methyl benzene methyl mercaptan and N, N-dimethylformamide are added into a reaction kettle, nitrogen is introduced for protection, carrying out reflux reaction for 7-9h at the rotation speed of 150-200r/min and the temperature of 120-130 ℃ to obtain an intermediate 8, adding the intermediate 8, iron powder and ethanol into a reaction kettle, carrying out reflux reaction for 3-5h at the temperature of 80-85 ℃, adding a hydrochloric acid solution for 20-30min, continuously reacting for 5-6h, and adjusting the pH value of the reaction solution to 7 to prepare an intermediate 9;
step A5: dissolving an intermediate 9 in tetrahydrofuran, introducing chlorine, reacting for 1-2h under the condition of illumination to obtain an intermediate 10, adding the intermediate 10, an intermediate 6 and dimethyl sulfoxide into a reaction kettle, adding 1-hydroxybenzotriazole under the conditions of a rotation speed of 150-, dissolving the intermediate 13 in tetrahydrofuran, adding boron tribromide at the temperature of 70-80 ℃ below zero, reacting for 10-15h at the temperature of 25-30 ℃ after the addition is finished, filtering to remove filtrate, and distilling the filtrate to remove tetrahydrofuran to obtain the antioxidant.
4. The vehicle paint maintenance coating agent of claim 3, wherein: the using amount ratio of the deionized water, the concentrated hydrochloric acid, the o-nitroaniline and the sodium nitrite in the step A1 is 5mL to 5.3mL to 2g to 1g, the mass fraction of the concentrated hydrochloric acid is 36%, and the using amount ratio of the sodium carbonate, the m-aminophenol and the diazo solution is 2.3g to 1.2g to 6 mL.
5. The vehicle paint maintenance coating agent of claim 3, wherein: the using amount ratio of the deionized water, the sodium hydroxide, the intermediate 1 and the thiourea dioxide in the step A2 is 150mL to 8g to 6.5g to 10 g.
6. The vehicle paint maintenance coating agent of claim 3, wherein: the molar ratio of the cyanuric chloride to the 5-methyl salicylic acid in the step A3 is 1:3, the amount of the aluminum trichloride is 10-15% of the mass of the 5-methyl salicylic acid, the molar ratio of the amount of the intermediate 3 to the amount of the intermediate 2 is 1:3, the amount of the 1-hydroxybenzotriazole is 35% of the mass of the intermediate 3, the amount of the intermediate 4, the potassium carbonate and the dimethyl sulfate is 3:1:4, and the amount ratio of the intermediate 5, the deionized water and the potassium permanganate is 2g:80 mL:5.
7. The vehicle paint maintenance coating agent of claim 3, wherein: the dosage ratio of the o-nitrophenol, the formaldehyde, the ethanol and the dimethylamine in the step A4 is 1mol:3mol:50mL:3mol, the dosage ratio of the intermediate 7, the p-methyl benzenethiol and the N, N-dimethylformamide is 0.5mol:1mol:100mL, the dosage ratio of the intermediate 8, the iron powder, the ethanol and the hydrochloric acid solution is 2g:4.5g:60mL:10mL, the volume fraction of the ethanol is 90%, the hydrochloric acid solution is concentrated hydrochloric acid with the mass fraction of 36% and ethanol with the volume fraction of 95% are mixed according to the volume ratio of 1: 9.
8. The vehicle paint maintenance coating agent of claim 3, wherein: the molar ratio of the intermediate 9 to the chlorine in the step A5 is 1:3, the molar ratio of the intermediate 10 to the intermediate 6 is 1:1, the amount of 1-hydroxybenzotriazole is 20-25% of the intermediate 10, the amount of diphenylamine, sulfur and iodine is 21.5:8:0.15, the molar ratio of the intermediate 11 to the intermediate 12 is 1:6, and the amount of the intermediate 7 to boron tribromide is 1g:5 mL.
9. The method for preparing the vehicle paint maintenance coating agent according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: adding tetraethoxysilane, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h under the conditions that the rotating speed is 200-300r/min and the temperature is 70-80 ℃ to prepare silica gel;
step S2: adding ethyl orthotitanate, half amount of ethanol and half amount of deionized water into a reaction kettle, and stirring for 3-5h at the rotation speed of 200-300r/min and the temperature of 80-85 ℃ to prepare titanium gel;
step S3: and (4) adding the silicon gel prepared in the step S1 and the titanium gel prepared in the step S2 into a stirring kettle, stirring for 1-1.5h under the condition that the rotating speed is 800r/min, adding an oxidation resistant agent and a film forming auxiliary agent, and continuously stirring for 2-3h to prepare the car paint maintenance coating agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113200942A (en) * | 2021-05-12 | 2021-08-03 | 上绍同烯达(绍兴)新材料科技有限公司 | Antioxidant and method for preparing antioxidant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113200942A (en) * | 2021-05-12 | 2021-08-03 | 上绍同烯达(绍兴)新材料科技有限公司 | Antioxidant and method for preparing antioxidant |
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