CN115746614A - Synthesis method of novel corrosion-resistant high-throwing-power cathode electrophoretic coating - Google Patents
Synthesis method of novel corrosion-resistant high-throwing-power cathode electrophoretic coating Download PDFInfo
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- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The invention discloses a novel synthesis method of a corrosion-resistant high-throwing-power cathode electrophoretic coating, which relates to the technical field of cathode electrophoretic coating production and comprises the following materials: 55-80 parts of main resin; 1-10 parts of blocked isocyanate curing agent; 20-35 parts of aqueous mercapto polyol modified epoxy resin; 1-10 parts of hydrogen-containing siloxane polymer; 1-10 parts of a modified polyethylene wax lotus leaf hydrophobing agent; 1-10 parts of an antishrinking agent of a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate; 1-10 anionic mineral modified rheological aid; 1-10 parts of modified imidazole and oxazolidine salt spray resistant auxiliary agent; 50-100 parts of color paste, the invention solves the problem that the surface of the traditional cathode electrophoretic coating is easy to form irregular small pits due to impurities after being dried in use, so that the shrinkage cavity is caused, the smoothness after film forming is lower, the hydrophobic effect, the wear-resisting effect and the corrosion-resisting effect are not ideal, the coating is easy to be polluted, scratched or corroded by external impurities, and the storage stability is poorer.
Description
Technical Field
The invention belongs to the field of production of cathode electrophoretic coatings, and particularly relates to a novel synthesis method of a corrosion-resistant high-throwing-power cathode electrophoretic coating.
Background
The cathode electrophoretic paint is a bi-component, one component is white uniform emulsion liquid, the other component is gray or black pigment slurry, the raw materials mainly comprise epoxy resin, ether alcohol compound, isocyanate and the like, the electrophoretic paint is from the 30 th century of 20 th century, the research on synthetic cationic resin is started from the middle of the 60 th century of 20 th century, the electrophoretic paint is used as a primer on household appliances with high requirements on corrosion resistance in the early 70 th of 20 th century, and then the cathode electrophoretic paint with higher corrosion resistance and decorative effect is gradually developed.
Because it has excellent anticorrosion, high swimming rate, high levelling property, high decorative and coating automation degree high, coating pollution characteristics such as being few, the wide application is in the automotive industry to popularize and apply to building materials, light industry, household electrical appliances and other industrial fields and hardware and handicraft surface anticorrosion and decoration, the technological process is: feeding → resin dissolution → epoxy amine addition → isocyanate blocking agent → resin neutralization → emulsification → component 1 emulsion; feeding → resin pigment → grinding and dispersing → adjusting → component 2 color paste, but the dried surface of the cathode electrophoretic coating prepared by the preparation method of the cathode electrophoretic coating in the prior art is easy to form irregular small pits due to impurities to cause the problem of shrinkage cavity when in use, so that the smoothness after film forming is lower, the hydrophobic effect, the wear-resistant effect and the corrosion-resistant effect are not ideal enough, the coating is easy to be polluted, scratched or corroded by external impurities, and the storage stability is poor.
Therefore, it is of great significance to research a new synthesis method of the corrosion-resistant high-throwing-power cathode electrophoretic coating to solve the problems.
Disclosure of Invention
The invention provides a novel synthesis method of a corrosion-resistant high-throwing-power cathode electrophoretic paint, which is used for solving the technical problems that after being dried, a cathode electrophoretic paint prepared by the preparation method of the cathode electrophoretic paint in the prior art is easy to form irregular small pits on the surface due to impurities, so that shrinkage cavities occur, the smoothness after film forming is lower, the hydrophobic effect, the wear-resistant effect and the corrosion-resistant effect are not ideal, the cathode electrophoretic paint is easy to be polluted, scratched or corroded by external impurities, and the storage stability is poorer.
In order to solve the technical problems, the invention provides a novel method for synthesizing a corrosion-resistant high-throwing-power cathode electrophoretic coating, which comprises the following materials:
55-80 parts of main resin; 1-10 parts of blocked isocyanate curing agent; 20-35 parts of aqueous mercapto polyol modified epoxy resin; 1-10 parts of hydrosiloxane polymer; 1-10 parts of a modified polyethylene wax lotus leaf hydrophobing agent; 1-10 parts of an antishrinking agent of a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate; 1-10 anionic mineral modified rheological aid; 1-10 parts of modified imidazole and oxazolidine salt spray resistant auxiliary agent; 50-100 parts of color paste;
the following preparation arrangement is also included:
step S01: putting the raw materials except the color paste into a dispersion kettle for uniform dispersion;
step S02: adjusting by using a pH regulator, and controlling the pH of the system to be between 5.3 and 6.5;
step S03: adding color paste and stirring uniformly;
step S04: detecting the fineness of the system and filtering.
Preferably, the material of the main resin includes a solvent, an initiator, a monomer and a neutralizing agent; the monomer comprises: isobornyl methacrylate, methyl methacrylate, styrene, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, butyl acrylate and phosphate ester monomers; the initiator comprises the following components: azobisisobutyronitrile; the solvent comprises: one or more of isopropanol, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethyl acetate, butyl acetate, ethylene glycol ethyl ether acetate and n-butanol; the neutralizing agent comprises: one of formic acid, acetic acid and lactic acid.
Preferably, the preparation step of the main resin comprises:
step T01: putting the solvent into a reactor with a stirring device, a dropping funnel, a cold air pipe and a thermometer, adding a specified amount of initiator and solvent, starting stirring, and heating to 80-100 ℃;
step T02: uniformly dripping the mixture of the reacted monomer and the initiator for 1 to 5 times, wherein the dripping time is 2 to 4 hours, and after the dripping is finished, keeping the temperature at 80 to 100 ℃ for 0.5 to 2.5 hours;
step T03: and (3) supplementing the rest initiator for 2 times at intervals of 0.5-2.5 hours, continuing to preserve heat for 0.5-2.5 hours after supplementing is finished, cooling after heat preservation is finished, adding a neutralizer, stirring, and discharging to obtain the main resin of the electrophoretic paint.
Preferably, the preparation method of the color paste comprises the following steps:
step U01: 229 parts by weight of deionized water is added into a reaction vessel with a stirring device, and the rotating speed is controlled to be 1200rpm;
step U02: adding 100 parts by weight of dispersion resin, uniformly dispersing, adding 69 parts by weight of modified alumina, 27 parts by weight of silane oligomer, 135 parts by weight of china clay, 21 parts by weight of carbon black, 4 parts by weight of dibutyltin oxide and 1 part by weight of wetting agent, and uniformly mixing;
step U03: grinding by a high-speed grinder for 2-3 hours at a controlled rotating speed of 3000rpm until the fineness is less than 15 mu m.
Preferably, the preparation method of the dispersion resin comprises:
step Y01: mixing a sulfhydryl compound, polyol, an inert solvent, a solid super acidic catalyst and an organic tin catalyst, then preserving the temperature for 7-8 hours at 160-200 ℃, then introducing inert gas at 150-160 ℃, and preserving the temperature for 1-2 hours at 150-160 ℃ to obtain a chain extender; the molar ratio of the mercapto compound to the polyol is 1.2-2.0;
step Y02: heating the chain extender obtained in the step Y01 and the epoxy resin to 100-110 ℃, adding a tertiary amine catalyst, then preserving heat for 0.5-1 h at 130-140 ℃, and then cooling to 90-100 ℃ and preserving heat for 1-2 h to obtain modified epoxy resin; the mass ratio of the epoxy resin to the chain extender is 0.5-10;
step Y03: heating the modified resin obtained in the step Y02 and an alcohol ether solvent to 80-100 ℃, then adding an organic amine compound, preserving the heat for 2-4 h at 100-120 ℃, then adding a cross-linking agent, mixing for 1-2 h at 70-110 ℃, then adding an organic acid or an inorganic acid, mixing for 1-2 h at 80-90 ℃ to obtain a product A, and then mixing the product A with water uniformly to obtain the modified resin.
Compared with the prior art, the invention has the following advantages:
1. the novel synthesis method of the corrosion-resistant high-throwing-power cathode electrophoretic paint has high salt spray resistance, can obtain a salt spray resistance effect of about 400-700 hours in a salt spray resistance test in a salt spray machine, greatly improves the salt spray resistance of a paint film of the electrophoretic paint, and further improves the quality of a processed product of the electrophoretic paint.
2. The novel synthesis method of the corrosion-resistant high-throwing-power cathode electrophoretic coating has the advantages of low baking temperature, low energy consumption, flat and smooth paint film appearance and high throwing power which is up to 0.65.
3. The novel synthesis method of the corrosion-resistant high-throwing-power cathode electrophoretic coating is simple in preparation method and convenient for batch production.
Drawings
FIG. 1 is a diagram of a method for preparing a novel corrosion-resistant high-throwing-power cathode electrophoretic coating according to the present invention;
FIG. 2 is a structural diagram of a preparation method of a main resin in a new synthesis method of a corrosion-resistant high-throwing-power cathode electrophoretic paint of the invention;
FIG. 3 is a structural diagram of a method for preparing color paste in a new method for synthesizing a corrosion-resistant high-throwing-power cathode electrophoretic paint of the invention;
FIG. 4 is a structural diagram of a method for preparing a dispersion resin in a new method for synthesizing a corrosion-resistant high-throwing-power cathode electrophoretic paint of the present invention;
Detailed Description
Referring to fig. 1-4, the present invention provides a technical solution: a new method for synthesizing a corrosion-resistant high-throwing-power cathode electrophoretic coating comprises the following materials: 55-80 parts of main resin; 1-10 parts of blocked isocyanate curing agent; 20-35 parts of aqueous mercapto polyol modified epoxy resin; 1-10 parts of hydrogen-containing siloxane polymer; 1-10 parts of a modified polyethylene wax lotus leaf hydrophobing agent; 1-10 parts of an antishrinking agent of a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate; 1-10 anionic mineral modified rheological aid; 1-10 parts of modified imidazole and oxazolidine salt spray resistant auxiliary agent; 50-100 parts of color paste; the following preparation arrangement is also included: step S01: putting the raw materials except the color paste into a dispersion kettle for uniform dispersion; step S02: adjusting by using a pH regulator, and controlling the pH of the system to be between 5.3 and 6.5; step S03: adding color paste and stirring uniformly; step S04: detecting the fineness of the system and filtering.
Further, the material of the main resin comprises a solvent, an initiator, a monomer and a neutralizing agent; the monomer comprises: isobornyl methacrylate, methyl methacrylate, styrene, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, butyl acrylate and phosphate ester monomers; the initiator comprises: azobisisobutyronitrile; the solvent comprises: one or more of isopropanol, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethyl acetate, butyl acetate, ethylene glycol ethyl ether acetate and n-butanol; the neutralizing agent comprises: one of formic acid, acetic acid and lactic acid.
Further, the preparation method of the main resin comprises the following steps:
step T01: putting the solvent into a reactor with a stirring device, a dropping funnel, a cold air pipe and a thermometer, adding a specified amount of initiator and solvent, starting stirring, and heating to 80-100 ℃;
step T02: uniformly dripping a mixture of the reacted monomer and the initiator for 1 to 5 times for 2 to 4 hours, and preserving the heat for 0.5 to 2.5 hours at the temperature of between 80 and 100 ℃ after finishing dripping;
step T03: and (3) supplementing the rest initiator for 2 times at intervals of 0.5-2.5 hours, continuing to preserve heat for 0.5-2.5 hours after supplementing is finished, cooling after heat preservation is finished, adding a neutralizer, stirring, and discharging to obtain the main resin of the electrophoretic paint.
Further, the preparation method of the color paste comprises the following steps:
step U01: 229 parts by weight of deionized water is added into a reaction vessel with a stirring device, and the rotating speed is controlled to be 1200rpm;
step U02: adding 100 parts by weight of dispersion resin, uniformly dispersing, adding 69 parts by weight of modified alumina, 27 parts by weight of silane oligomer, 135 parts by weight of china clay, 21 parts by weight of carbon black, 4 parts by weight of dibutyltin oxide and 1 part by weight of wetting agent, and uniformly mixing;
step U03: grinding by a high-speed grinder for 2-3 hours at a controlled rotating speed of 3000rpm until the fineness is less than 15 mu m.
Further, the preparation method of the dispersion resin comprises the following steps:
step Y01: mixing a sulfhydryl compound, polyol, an inert solvent, a solid super acidic catalyst and an organic tin catalyst, then preserving the temperature for 7-8 hours at 160-200 ℃, then introducing inert gas at 150-160 ℃, and preserving the temperature for 1-2 hours at 150-160 ℃ to obtain a chain extender; the molar ratio of the mercapto compound to the polyol is 1.2-2.0;
step Y02: heating the chain extender obtained in the step Y01 and the epoxy resin to 100-110 ℃, adding a tertiary amine catalyst, then preserving heat for 0.5-1 h at 130-140 ℃, and then cooling to 90-100 ℃ and preserving heat for 1-2 h to obtain modified epoxy resin; the mass ratio of the epoxy resin to the chain extender is 0.5-10;
step Y03: heating the modified resin obtained in the step Y02 and an alcohol ether solvent to 80-100 ℃, then adding an organic amine compound, preserving heat for 2-4 h at 100-120 ℃, then adding a cross-linking agent, mixing for 1-2 h at 70-110 ℃, then adding an organic acid or an inorganic acid, mixing for 1-2 h at 80-90 ℃ to obtain a product A, and then mixing the product A with water uniformly to obtain the modified resin.
In the embodiment, the cathode electrophoretic coating has high salt spray resistance, can obtain a salt spray resistance effect of about 400-700 hours in a salt spray resistance test in a salt spray machine, greatly improves the salt spray resistance of a paint film of the electrophoretic paint coating, further improves the quality of a processed product of the electrophoretic paint, has low baking temperature and low energy consumption, has flat and smooth appearance of the paint film, high throwing power up to 0.65, is simple in preparation method, and is convenient for batch production.
Claims (5)
1. A new method for synthesizing corrosion-resistant high-throwing-power cathode electrophoretic paint is characterized by comprising the following steps: comprises the following materials:
55-80 parts of main resin; 1-10 parts of blocked isocyanate curing agent; 20-35 parts of aqueous mercapto polyol modified epoxy resin; 1-10 parts of hydrogen-containing siloxane polymer; 1-10 parts of a modified polyethylene wax lotus leaf hydrophobing agent; 1-10 parts of an anti-shrinking agent of a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate; 1-10 anionic mineral modified rheological aid; 1-10 parts of modified imidazole and oxazolidine salt spray resistant auxiliary agent; 50-100 parts of color paste;
the following preparation arrangement is also included:
step S01: putting the raw materials except the color paste into a dispersion kettle for uniform dispersion;
step S02: adjusting by using a pH regulator, and controlling the pH of the system to be between 5.3 and 6.5;
step S03: adding color paste and stirring uniformly;
step S04: detecting the fineness of the system and filtering.
2. The method for synthesizing the novel corrosion-resistant high-throwing-power cathodic electrophoretic paint according to claim 1, wherein the materials of the main resin comprise a solvent, an initiator, a monomer and a neutralizing agent; the monomer comprises: isobornyl methacrylate, methyl methacrylate, styrene, hydroxyethyl methacrylate, dimethylaminoethyl methacrylate, butyl acrylate and phosphate ester monomers; the initiator comprises: azobisisobutyronitrile; the solvent comprises: one or more of isopropanol, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethyl acetate, butyl acetate, ethylene glycol ethyl ether acetate and n-butanol; the neutralizing agent comprises: one of formic acid, acetic acid and lactic acid.
3. The method for synthesizing the novel corrosion-resistant high-throwing-power cathodic electrophoretic coating according to claim 2, wherein the preparation of the main resin comprises the following steps:
step T01: putting the solvent into a reactor with a stirring device, a dropping funnel, a cold air pipe and a thermometer, adding a specified amount of initiator and solvent, starting stirring, and heating to 80-100 ℃;
step T02: uniformly dripping the mixture of the reacted monomer and the initiator for 1 to 5 times, wherein the dripping time is 2 to 4 hours, and after the dripping is finished, keeping the temperature at 80 to 100 ℃ for 0.5 to 2.5 hours;
step T03: and adding the rest initiator for one time at intervals of 0.5-2.5 hours for 2 times, continuously preserving the temperature for 0.5-2.5 hours after the addition is finished, cooling after the heat preservation is finished, adding a neutralizing agent, stirring, and discharging to obtain the main resin of the electrophoretic paint.
4. The synthesis method of the novel corrosion-resistant high-throwing-power cathode electrophoretic paint as claimed in claim 1, wherein the preparation method of the color paste comprises the following steps:
step U01: 229 parts by weight of deionized water is added into a reaction vessel with a stirring device, and the rotating speed is controlled to be 1200rpm;
step U02: adding 100 parts by weight of dispersion resin, uniformly dispersing, adding 69 parts by weight of modified alumina, 27 parts by weight of silane oligomer, 135 parts by weight of china clay, 21 parts by weight of carbon black, 4 parts by weight of dibutyltin oxide and 1 part by weight of wetting agent, and uniformly mixing;
step U03: grinding by a high-speed grinder for 2-3 hours at a controlled rotating speed of 3000rpm until the fineness is less than 15 mu m.
5. The method for synthesizing the novel corrosion-resistant high-throwing-power cathode electrophoretic coating according to claim 4, wherein the preparation method of the dispersion resin comprises the following steps:
step Y01: mixing a sulfhydryl compound, polyol, an inert solvent, a solid super acidic catalyst and an organic tin catalyst, then preserving the temperature for 7-8 hours at 160-200 ℃, then introducing inert gas at 150-160 ℃, and preserving the temperature for 1-2 hours at 150-160 ℃ to obtain a chain extender; the molar ratio of the mercapto compound to the polyol is 1.2-2.0;
step Y02: heating the chain extender obtained in the step Y01 and the epoxy resin to 100-110 ℃, adding a tertiary amine catalyst, then preserving heat for 0.5-1 h at 130-140 ℃, and then cooling to 90-100 ℃ and preserving heat for 1-2 h to obtain modified epoxy resin; the mass ratio of the epoxy resin to the chain extender is 0.5-10;
step Y03: heating the modified resin obtained in the step Y02 and an alcohol ether solvent to 80-100 ℃, then adding an organic amine compound, preserving heat for 2-4 h at 100-120 ℃, then adding a cross-linking agent, mixing for 1-2 h at 70-110 ℃, then adding an organic acid or an inorganic acid, mixing for 1-2 h at 80-90 ℃ to obtain a product A, and then mixing the product A with water uniformly to obtain the modified resin.
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| CN103865360A (en) * | 2014-03-28 | 2014-06-18 | 湖南伟邦汽车涂料有限公司 | Acid-proof cathode electrophoretic paint as well as preparation method and application method |
| CN108976981A (en) * | 2018-06-11 | 2018-12-11 | 中海油常州涂料化工研究院有限公司 | A kind of cathode electrophoresis dope lotion and preparation method thereof, cathode electrophoresis dope and preparation method thereof |
| CN110117339A (en) * | 2019-06-13 | 2019-08-13 | 深圳市志邦科技有限公司 | A kind of ability cathode electrophoresis coating resins of high salt spray resistance and preparation method thereof |
| CN112552785A (en) * | 2020-12-03 | 2021-03-26 | 上海瑞君电泳涂料有限公司 | Anti-shrinkage cathode electrophoretic coating composition and preparation method thereof |
| CN114316661A (en) * | 2022-01-07 | 2022-04-12 | 枣阳市旺前电泳涂料有限公司 | Synthesis method of corrosion-resistant high-throwing-power film type cathode electrophoretic paint |
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2022
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| CN103865360A (en) * | 2014-03-28 | 2014-06-18 | 湖南伟邦汽车涂料有限公司 | Acid-proof cathode electrophoretic paint as well as preparation method and application method |
| CN108976981A (en) * | 2018-06-11 | 2018-12-11 | 中海油常州涂料化工研究院有限公司 | A kind of cathode electrophoresis dope lotion and preparation method thereof, cathode electrophoresis dope and preparation method thereof |
| CN110117339A (en) * | 2019-06-13 | 2019-08-13 | 深圳市志邦科技有限公司 | A kind of ability cathode electrophoresis coating resins of high salt spray resistance and preparation method thereof |
| CN112552785A (en) * | 2020-12-03 | 2021-03-26 | 上海瑞君电泳涂料有限公司 | Anti-shrinkage cathode electrophoretic coating composition and preparation method thereof |
| CN114316661A (en) * | 2022-01-07 | 2022-04-12 | 枣阳市旺前电泳涂料有限公司 | Synthesis method of corrosion-resistant high-throwing-power film type cathode electrophoretic paint |
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