CN114921775A - Environment-friendly coating agent and preparation method thereof - Google Patents
Environment-friendly coating agent and preparation method thereof Download PDFInfo
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- CN114921775A CN114921775A CN202210531101.6A CN202210531101A CN114921775A CN 114921775 A CN114921775 A CN 114921775A CN 202210531101 A CN202210531101 A CN 202210531101A CN 114921775 A CN114921775 A CN 114921775A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
The invention discloses an environment-friendly coating agent and a preparation method thereof, and relates to the technical field of coating agents. An environment-friendly coating agent is prepared from the following raw materials in parts by weight: 20-30 parts of silicate, 1-5 parts of organic silane resin, 0.5-0.85 part of anticorrosive additive, 10-12 parts of silane coupling agent, 7-13 parts of unsaturated polyester modified acrylic resin, 1.1-1.8 parts of calcium-zinc stabilizer, 0.8-1.3 parts of modified nano silicon dioxide, 0.9-1.4 parts of copper dialkyl dithiophosphate antioxidant, 60-80 parts of propylene glycol and 40-55 parts of deionized water. The invention provides an environment-friendly nano coating agent, which belongs to a phosphorus, chromium and nickel-free environment-friendly pretreatment agent, is economical to use, simple to operate, can be formed at room temperature without wastewater treatment cost, can form a nano ceramic coating by adding nano silicon dioxide and modifying the nano silicon dioxide, greatly improves the corrosion resistance, has environment-friendly capability and simultaneously has the corrosion resistance greater than that of phosphating solution.
Description
Technical Field
The invention relates to the technical field of coating agents, in particular to an environment-friendly coating agent and a preparation method thereof.
Background
The coating agent is a metal surface treating agent, can react with metal, can form a protective film which is insoluble in water, chemically inert and firmly attached to the metal surface while removing rust on the metal surface, is favorable for preventing metal oxidation, and is also favorable for enhancing the bonding force and adhesive force of a sprayed paint film, plastic powder and metal in the subsequent metal surface spraying process, so that the coating agent is widely used in the manufacturing industries of metal products such as automobiles, refrigerators, air conditioners and the like. The coating agent comprises phosphorus-containing coating agent and phosphorus-free coating agent, the phosphorus-containing coating agent has serious pollution to the environment, a large amount of phosphate-containing wastewater and waste residues are generated in the using process, the treatment process of the wastewater and the waste residues is complex, and the treatment cost is high.
The existing chromizing liquid contains harmful heavy metals such as chromium, nickel and the like which seriously harm the environment, and the wastewater treatment cost is high; the main components of the phosphating solution are phosphoric acid and zinc oxide, the wastewater contains a large amount of phosphide and zinc, the wastewater discharge needs to be processed in an environment-friendly way, and meanwhile, the phosphating solution belongs to a reactive coating agent and generates a large amount of residues in the film forming process.
Disclosure of Invention
The invention aims to provide an environment-friendly coating agent and a preparation method thereof, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an environment-friendly coating agent is prepared from the following raw materials in parts by weight: 20-30 parts of silicate, 1-5 parts of organosilane resin, 0.5-0.85 part of anticorrosive additive, 10-12 parts of silane coupling agent, 7-13 parts of unsaturated polyester modified acrylic resin, 1.1-1.8 parts of calcium-zinc stabilizer, 0.8-1.3 parts of modified nano silicon dioxide, 0.9-1.4 parts of copper dialkyl dithiophosphate antioxidant, 60-80 parts of propylene glycol and 40-55 parts of deionized water.
A preparation method of an environment-friendly coating agent comprises the following steps:
step one, preparing nano silicon dioxide; modifying the nano silicon dioxide to obtain modified nano silicon dioxide;
step two, preparing silane hydrolysate, adding propylene glycol and deionized water into the preparation device, dripping the silane coupling agent into the preparation device under the stirring condition of the rotation speed of 800-;
step three, preparing the silane unsaturated polyester modified acrylic resin, putting the unsaturated polyester modified acrylic resin into preparation equipment, and stirring the silane hydrolysate and the unsaturated polyester modified acrylic resin for 2 hours under the condition that the rotation speed is 1000-1200rpm to obtain the silane unsaturated polyester modified acrylic resin;
step four: adding deionized water into the reaction kettle, then adding silicate, a stabilizing agent, an anticorrosive additive and an antioxidant, and uniformly stirring;
step five: and continuously adding propylene glycol, organic silane resin, silane hydrolysate, silane unsaturated polyester modified acrylic resin and modified nano silicon dioxide into the reaction kettle, uniformly stirring, stirring for 10-25 minutes, sampling, analyzing and packaging qualified products.
As a preferred technical scheme in the application, the method for preparing the nano-silica in the first step comprises the steps of adding 40-55 parts of absolute ethyl alcohol, 10-20 parts of deionized water and 1.3-2.5 parts of 25-28% by mass of concentrated ammonia water into an erlenmeyer flask, placing the erlenmeyer flask into a magnetic stirrer, stirring for 10-15min under the condition of 900rpm, then adding 0.8-1.2 parts of tetraethoxysilane and 37 parts of absolute ethyl alcohol into the erlenmeyer flask, stirring for 1-2min under the condition of 1000rpm, reducing the rotation speed to 600-700rpm after stirring is finished, tightly covering a bottle stopper, keeping the reaction temperature between 20-30 ℃, continuously reacting for 2-3h, after the reaction is finished, carrying out centrifugal separation and collection on the solution in the erlenmeyer flask, respectively washing the collected solid for 2-3 times by using the absolute ethyl alcohol and the deionized water, and drying the obtained solid in a drying box, and grinding to obtain the nano silicon dioxide powder.
As a preferred technical scheme in the application, the step of modifying the nano-silica comprises the steps of adding a certain amount of isopropanol into nano-silica powder, and then putting the mixture into a stirrer to be uniformly stirred to obtain mixed nano-silica powder; weighing a titanate coupling agent with the powder mass of 10%, dissolving the titanate coupling agent in a certain amount of isopropanol, then placing the mixture in an ultrasonic generator, carrying out ultrasonic treatment for a certain time, adding mixed nano-silica powder, then stirring at a high speed for 30 minutes, raising the temperature to 80 ℃, continuing to carry out ultrasonic solvent volatilization for 30 minutes, then placing the mixture in a vacuum oven at 80 ℃ for drying, grinding and sieving for later use to obtain modified nano-silica powder, and then carrying out post-treatment on the modified nano-silica powder to obtain modified nano-silica.
In the second step, the silane coupling agent is one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, and methyltrimethoxysilane.
As a preferable technical scheme in the application, the antioxidant in the fourth step is one of organic copper carboxylate, copper thiocarbamate or copper dialkyl dithiophosphate.
As a preferred technical scheme in the application, the stabilizing agent in the fourth step is a calcium zinc stabilizing agent.
As a preferred technical scheme in the application, the preparation method of the preservative additive in the fourth step comprises the following steps: the polyborosiloxane was dissolved in dimethyl sulfoxide to give a solution and stirred at high speed for at least 2 h.
Compared with the prior art, the invention has the beneficial effects that:
the environment-friendly coating agent and the preparation method thereof provide the environment-friendly nano coating agent, belong to environment-friendly pretreatment agents without phosphorus, chromium and nickel, are economical to use, simple to operate, and molded at room temperature, do not need wastewater treatment cost, and form a nano ceramic coating by adding nano silicon dioxide and modifying the nano silicon dioxide, so that the corrosion resistance of the nano ceramic coating is greatly improved, and the nano ceramic coating has environment-friendly capability and is higher than phosphating solution in corrosion resistance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows: step one, adding 30 parts of absolute ethyl alcohol, 13 parts of deionized water and 2.5 parts of 29% concentrated ammonia water by mass into a conical flask, placing the conical flask into a magnetic stirrer, stirring for 10min under the condition of 900rpm, then adding 1.6 parts of tetraethoxysilane and 32 parts of absolute ethyl alcohol into the conical flask, stirring for 2min under the condition of 1000rpm, reducing the rotation speed to 700rpm after stirring, tightly covering a bottle stopper, keeping the reaction temperature between 20 and 30 ℃, continuously reacting for 2h, centrifugally separating and collecting the solution in the conical flask after the reaction is finished, respectively cleaning the collected solid for 2 times by using the absolute ethyl alcohol and the deionized water, placing the obtained solid into a drying box for drying treatment, grinding to obtain nano silicon dioxide powder, adding a certain amount of isopropanol into the nano silicon dioxide powder, placing into the stirrer again, and stirring uniformly, obtaining mixed nano silicon dioxide powder; weighing titanate coupling agent with the powder mass of 10%, dissolving the titanate coupling agent in a certain amount of isopropanol, placing the mixture in an ultrasonic generator, carrying out ultrasonic treatment for a certain time, adding mixed nano-silica powder, stirring at a high speed for 30 minutes, heating to 80 ℃, continuing to ultrasonically volatilize the solvent for 30 minutes, then placing the mixture in a vacuum oven at 80 ℃ for drying, grinding and sieving for later use to obtain modified nano-silica powder, and then carrying out post-treatment on the modified nano-silica powder to obtain modified nano-silica.
Step two, preparing silane hydrolysate, namely adding propylene glycol and deionized water into a preparation device, dripping methyltrimethoxysilane into preparation equipment under the stirring condition of the rotation speed of 900rpm, placing the equipment at room temperature, and hydrolyzing for 48 hours under the condition of maintaining the stirring rotation speed of 900rpm to obtain the silane hydrolysate;
step three, preparing silane unsaturated polyester modified acrylic resin, putting the unsaturated polyester modified acrylic resin into preparation equipment, and stirring silane hydrolysate and the unsaturated polyester modified acrylic resin for 2 hours under the condition that the rotating speed is 1000rpm to obtain the silane unsaturated polyester modified acrylic resin;
step four: dissolving polyborosiloxane in dimethyl sulfoxide to obtain a solution, stirring at a high speed for 2.5 hours to obtain an anticorrosive additive, adding 40 parts of deionized water into a reaction kettle, then adding 30 parts of silicate, 1.2 parts of calcium-zinc stabilizer, 0.6 part of anticorrosive additive and 0.9 part of organic copper carboxylate, and stirring uniformly;
step five: and continuously adding 60 parts of propylene glycol, 4 parts of organic silane resin, 8 parts of silane hydrolysate, 10 parts of silane unsaturated polyester modified acrylic resin and 1.2 parts of modified nano silicon dioxide into the reaction kettle, uniformly stirring for 25 minutes, sampling, analyzing and packaging qualified products.
Example two: adding 30 parts of absolute ethyl alcohol, 13 parts of deionized water and 2.5 parts of 29% concentrated ammonia water into a conical flask, placing the conical flask into a magnetic stirrer, stirring for 10min at the rotating speed of 900rpm, then adding 1.6 parts of tetraethoxysilane and 32 parts of absolute ethyl alcohol into the conical flask, stirring for 2min at the rotating speed of 1000rpm, reducing the rotating speed to 700rpm after stirring, tightly covering a bottle stopper, keeping the reaction temperature between 20 and 30 ℃, continuously reacting for 2h, after the reaction is finished, centrifugally separating and collecting the solution in the conical flask, respectively washing the collected solid for 2 times by using the absolute ethyl alcohol and the deionized water, drying the obtained solid in a drying box, and grinding to obtain the nano silicon dioxide powder.
Example three: the first to fourth steps are the same as the first embodiment, and the parameters of the fifth step are modified, wherein 45 parts of propylene glycol, 3 parts of organosilane resin, 6 parts of silane hydrolysate, 8 parts of silane unsaturated polyester modified acrylic resin and 0.8 part of modified nano silicon dioxide are uniformly stirred.
Example four: the first to fourth steps are the same as the first embodiment, and the parameters of the fifth step are modified, wherein 50 parts of propylene glycol, 2 parts of organosilane resin, 4 parts of silane hydrolysate, 6 parts of silane unsaturated polyester modified acrylic resin and 0.7 part of modified nano silicon dioxide are uniformly stirred.
Example five: the first, second, third and fifth steps are the same as the first example, and the parameters of the fourth step are modified, specifically, 30 parts of ionized water, 20 parts of silicate, 0.8 part of calcium zinc stabilizer, 0.4 part of preservative additive and 0.5 part of organic copper carboxylate are added.
Example six: the first, second, third and fifth steps are the same as the first step, and the parameters of the fourth step are modified, specifically, 35 parts of ionized water, and then 25 parts of silicate, 1.1 parts of calcium zinc stabilizer, 0.6 part of preservative additive and 0.75 part of organic copper carboxylate are added.
Comparative example one: the comparative example is different from example 1 in that a commercially available coating agent, specifically, a chromium-free aluminum coating agent, brand Chang He, cat # CH-600, was used in the comparative example.
Comparative example two: the comparative example differs from example 1 in that a commercially available coating agent, specifically brand weiqi, cat # HWJ-248, zinc phosphating solution was used.
Respectively counting the coating agents prepared in the first to sixth examples and the first to second comparative examples as samples I to VI and comparative samples I to II, and firstly diluting the samples I to VI and the comparative samples I to II by 10-15 times with water for later use; firstly, washing the surface of an iron piece by using a weakly alkaline or weakly acidic washing liquid to remove oil stain and dust on the surface of an iron matrix, then washing other impurities remained on the surface of the iron piece by using water, directly soaking the iron piece in a diluent of a first to sixth sample and a first to second comparative sample, wherein the passivation temperature is 35-50 ℃, the passivation time is 35-55 s, drying at the temperature of 100-105 ℃, and drying at normal temperature; the specific test results of the corrosion resistance of the passive film are evaluated by performing a neutral salt spray test and are shown in the table.
As can be seen from the above table, the coating agents of samples one, three to six have excellent acid resistance and alkali resistance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. An environment-friendly coating agent is characterized in that: the coating agent is prepared from the following raw materials in parts by weight: 20-30 parts of silicate, 1-5 parts of organic silane resin, 0.5-0.85 part of anticorrosive additive, 10-12 parts of silane coupling agent, 7-13 parts of unsaturated polyester modified acrylic resin, 1.1-1.8 parts of calcium-zinc stabilizer, 0.8-1.3 parts of modified nano silicon dioxide, 0.9-1.4 parts of copper dialkyl dithiophosphate antioxidant, 60-80 parts of propylene glycol and 40-55 parts of deionized water.
2. A preparation method of an environment-friendly coating agent is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing nano silicon dioxide; modifying the nano silicon dioxide to obtain modified nano silicon dioxide;
step two, preparing silane hydrolysate, adding propylene glycol and deionized water into the preparation device, dripping the silane coupling agent into the preparation device under the stirring condition of the rotation speed of 800-;
step three, preparing the silane unsaturated polyester modified acrylic resin, putting the unsaturated polyester modified acrylic resin into preparation equipment, and stirring the silane hydrolysate and the unsaturated polyester modified acrylic resin for 2 hours under the condition that the rotation speed is 1000-1200rpm to obtain the silane unsaturated polyester modified acrylic resin;
step four: adding deionized water into the reaction kettle, then adding silicate, a stabilizing agent, an anticorrosive additive and an antioxidant, and uniformly stirring;
step five: and continuously adding propylene glycol, organic silane resin, silane hydrolysate, silane unsaturated polyester modified acrylic resin and modified nano silicon dioxide into the reaction kettle, uniformly stirring, stirring for 10-25 minutes, sampling, analyzing and packaging qualified products.
3. The method for preparing the environment-friendly film coating agent according to claim 2, characterized in that: the method for preparing the nano silicon dioxide in the first step comprises the steps of adding 40-55 parts of absolute ethyl alcohol, 10-20 parts of deionized water and 1.3-2.5 parts of 25-28% concentrated ammonia water by mass fraction into a conical flask, placing the conical flask into a magnetic stirrer, stirring for 10-15min at the rotation speed of 900rpm, then adding 0.8-1.2 parts of tetraethoxysilane and 37 parts of absolute ethyl alcohol into the conical flask, stirring for 1-2min at the rotation speed of 1000rpm, reducing the rotation speed to 600-700rpm after stirring, tightly covering a bottle stopper, keeping the reaction temperature between 20-30 ℃, continuously reacting for 2-3h, carrying out centrifugal separation and collection on the solution in the conical flask after the reaction is finished, respectively cleaning the collected solid for 2-3 times by using the absolute ethyl alcohol and the deionized water, placing the obtained solid into a drying box for drying treatment, grinding to obtain the nano silicon dioxide powder.
4. The method for preparing an environment-friendly film coating agent according to claim 2, wherein the method comprises the following steps: the step of modifying the nano silicon dioxide is to add a certain amount of isopropanol into the nano silicon dioxide powder and then put the nano silicon dioxide powder into a stirrer to be uniformly stirred to obtain mixed nano silicon dioxide powder; weighing titanate coupling agent with the powder mass of 10%, dissolving the titanate coupling agent in a certain amount of isopropanol, placing the mixture in an ultrasonic generator, carrying out ultrasonic treatment for a certain time, adding mixed nano-silica powder, stirring at a high speed for 30 minutes, heating to 80 ℃, continuing to ultrasonically volatilize the solvent for 30 minutes, then placing the mixture in a vacuum oven at 80 ℃ for drying, grinding and sieving for later use to obtain modified nano-silica powder, and then carrying out post-treatment on the modified nano-silica powder to obtain modified nano-silica.
5. The method for preparing the environment-friendly film coating agent according to claim 2, characterized in that: and in the second step, the silane coupling agent is one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane or methyltrimethoxysilane.
6. The method for preparing an environment-friendly film coating agent according to claim 2, wherein the method comprises the following steps: and in the fourth step, the antioxidant is one of organic copper carboxylate, copper thiocarbamate or copper dialkyl dithiophosphate.
7. The method for preparing an environment-friendly film coating agent according to claim 2, wherein the method comprises the following steps: and the stabilizer in the fourth step is a calcium zinc stabilizer.
8. The method for preparing the environment-friendly film coating agent according to claim 2, characterized in that: the preparation method of the anticorrosive additive in the fourth step comprises the following steps: the polyborosiloxane was dissolved in dimethyl sulfoxide to give a solution and stirred at high speed for at least 2 h.
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Cited By (1)
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| CN115287643A (en) * | 2022-08-23 | 2022-11-04 | 上海钱洪化学科技有限公司 | Silane coating agent and preparation method thereof |
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