CN115572545A - High-gloss electrosilvering coating composition, electrosilvering coating and preparation method thereof - Google Patents

High-gloss electrosilvering coating composition, electrosilvering coating and preparation method thereof Download PDF

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Publication number
CN115572545A
CN115572545A CN202110685784.6A CN202110685784A CN115572545A CN 115572545 A CN115572545 A CN 115572545A CN 202110685784 A CN202110685784 A CN 202110685784A CN 115572545 A CN115572545 A CN 115572545A
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resin
gloss
electrosilvering
silver
coating composition
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Inventor
马永强
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Langfang Nippon Paint Co ltd
Tianjin Binhai New Area Libang Paint Co ltd
Guangzhou Nippon Paint Co Ltd
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Langfang Nippon Paint Co ltd
Tianjin Binhai New Area Libang Paint Co ltd
Guangzhou Nippon Paint Co Ltd
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Priority to CN202110685784.6A priority Critical patent/CN115572545A/en
Publication of CN115572545A publication Critical patent/CN115572545A/en
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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
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/38—Paints containing free metal not provided for above in groups C09D5/00 - C09D5/36
    • 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
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0812—Aluminium

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention discloses a high-gloss electrosilvering coating composition, which is characterized by comprising the following components in percentage by weight: 1.8-2.2% of silver-aluminum electroplating slurry; 4.0-6.0% of electroplating silver resin; 0.04 to 0.06 percent of hydroxyl hyperbranched resin; 0.3 to 0.5 percent of blocked isocyanate resin; 0.03-0.05% of silver dropping prevention auxiliary agent; 0.08 to 0.13 percent of auxiliary agent; 91.0-93.0% of solvent. The silver electroplating coating composition is matched with black primer and varnish for use, the 20-degree gloss of a composite coating is more than 230, the gloss of the composite coating is far higher than that of the conventional silver electroplating coating composition, the 20-degree gloss of the composite coating is in a range of 170-180 degrees, the water resistance and the recoating performance are qualified, and the silver electroplating coating composition can be matched with liquid varnish or powder varnish for use. The invention also discloses an electro-silvering coating containing the electro-silvering coating composition, and a preparation method and application thereof.

Description

High-gloss electrosilvering coating composition, electrosilvering coating and preparation method thereof
Technical Field
The invention relates to the technical field of automobile coatings. And more particularly, to a high-gloss electro-silvering paint composition, an electro-silvering paint and a preparation method thereof.
Background
In recent years, with the rapid development of the automobile industry, the color appearance of the related matching products such as automobile hubs and the like also shows diversified requirements, such as electroplated hubs and silver-plated paint hubs. Compared with the automobile hub coated with the traditional paint, the electroplated hub and the wheel hub coated with the electroplated silver paint have high gloss and metal texture, and are popular with consumers. The glossiness of the electroplated wheel hub is higher than that of an electroplated silver paint wheel hub, the electroplated wheel hub process comprises water electroplating and vacuum electroplating, and the water and electricity wheel hub electroplating process has the defects of difficulty in treatment of generated wastewater and environmental pollution; the baking temperature of the medium paint layer of the vacuum plating wheel hub is high-temperature baking at 220-230 ℃, and the high-temperature baking can influence the mechanical strength and the like of the aluminum alloy wheel hub, so that the large-scale application of the plating wheel hub is limited.
Therefore, it is necessary to provide a high gloss electro-silvered coating composition and a preparation method thereof, and the composition can be matched with liquid varnish and powder varnish for use.
Disclosure of Invention
The first object of the present invention is to provide a high-gloss electrosilvering coating composition. The silver electroplating coating composition is matched with black primer and varnish for use, the 20-degree gloss of a composite coating is more than 230, the gloss of the composite coating is far higher than that of the conventional silver electroplating coating composition, the 20-degree gloss of the composite coating is in a range of 170-180 degrees, the water resistance and the recoating performance are qualified, and the silver electroplating coating composition can be matched with liquid varnish or powder varnish for use.
The second purpose of the invention is to provide a high-gloss electrosilvering paint.
The third purpose of the invention is to provide a preparation method of the high-gloss electrosilvering coating.
The fourth purpose of the invention is to provide the application of the high-gloss electrosilvering paint.
In order to achieve the first purpose, the invention adopts the following technical scheme:
a high-gloss electrosilvering coating composition comprises the following components in percentage by weight:
Figure BDA0003124558440000011
further, the particle size of the aluminum powder in the silver electroplating aluminum paste is 8-14 μm, and the non-volatile content of the silver electroplating aluminum paste is 9.90-10.10%.
Further, the content of non-volatile parts of the silver electroplating resin is 7.5-8.5%, and the Gardner viscosity is W-Z3.
Furthermore, the hydroxyl hyperbranched resin has the non-volatile content of 53.0-63.0%, the viscosity of 150-550mPa.s @25 ℃, and the hydroxyl content of 4.8-6.3% calculated by solid resin.
Furthermore, the non-volatile content of the blocked isocyanate resin is 73.0-77.0%, the unblocking temperature is 110-150 ℃, and the content of blocked isocyanate functional groups in the blocked isocyanate resin is 8-12 wt%.
Furthermore, the silver drop prevention auxiliary agent is a low-acidity modified polyester compound, and the nonvolatile content of the silver drop prevention auxiliary agent is 78.0-82.0%.
Further, the auxiliary agent is selected from one or more of a leveling agent, an ultraviolet absorber, a light stabilizer, a coupling agent or a wetting dispersant.
Further, the assistant comprises the following components in percentage by weight based on the total weight of the electroplated silver coating composition:
Figure BDA0003124558440000021
further, the solvent is selected from one or more of ketone solvents, ester solvents and aromatic hydrocarbon solvents.
Further, the ester solvent is selected from one or more of propylene glycol methyl ether acetate, ethyl 3-ethoxypropionate, butyl propionate, butyl acetate and ethyl acetate, and the ester solvent accounts for 56.0-60.0% of the total weight of the electrosilvering coating composition.
Further, the ketone solvent is selected from one or more of cyclohexanone, methyl amyl ketone, methyl isoamyl ketone and methyl isobutyl ketone, and the ketone solvent accounts for 16.0-20.0% of the total weight of the electrosilvering coating composition.
Further, the aromatic hydrocarbon solvent is selected from one or more of xylene, S-100#, S-150#, and the aromatic hydrocarbon solvent accounts for 14.0-18.0% of the total weight of the electrosilvering coating composition.
In order to achieve the second purpose, the invention adopts the following technical scheme:
a high-gloss electro-silvering paint whose raw material comprises the high-gloss electro-silvering paint composition as described in the first object above.
In order to achieve the third purpose, the invention adopts the following technical scheme:
a preparation method of high-gloss electrosilvering paint comprises the following steps:
1) Passivating the silver-electroplating aluminum paste to obtain passivated silver-electroplating aluminum paste;
2) Dissolving hydroxyl hyperbranched resin and blocked isocyanate resin in a part of solvent, and uniformly mixing to obtain a mixed resin semi-finished product;
3) And uniformly mixing the silver electroplating resin and the passivated silver electroplating aluminum paste, mixing the mixture with the semi-finished product of the mixed resin, and adding an auxiliary agent and the residual solvent to obtain the high-gloss silver electroplating coating.
In order to achieve the fourth object, the invention also protects the application of the high-gloss electrosilvering paint with the second object in the coating of the automobile hub.
The invention has the following beneficial effects:
in the high-gloss electrosilvering coating composition provided by the invention, specially selected electrosilvering resin is electrosilvering aluminum powder oriented resin, hydroxyl hyperbranched resin and blocked isocyanate resin are used as crosslinking curing resin, and proper auxiliaries are matched and used in the high-gloss electrosilvering coating, the prepared high-gloss electrosilvering coating composition is matched with black primer and varnish for use, the 20-degree gloss of a composite coating is more than 230, the gloss of the composite coating is far higher than that of the conventional electrosilvering coating composition by 20 degrees and is 170-180, the water resistance and the recoating performance are qualified, and the high-gloss electrosilvering coating composition can be matched with liquid varnish or powder varnish for use. The high-gloss electrosilvering coating provided by the invention can be well applied to the coating of automobile hubs.
Detailed Description
In order to more clearly illustrate the present invention, the present invention is further described below in conjunction with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
In order to solve the problems that the existing electroplating hub in the automobile hub electroplating process is not environment-friendly and affects the performance of the hub, the invention provides a high-gloss electrosilvering coating composition, which comprises the following components in percentage by weight:
Figure BDA0003124558440000031
in the electrosilvering coating composition, specially selected electrosilvering resin is electrosilvering aluminum powder oriented resin, hydroxyl hyperbranched resin and blocked isocyanate resin are combined as crosslinking curing resin, the addition amount of each component is controlled, and proper auxiliary agents are matched for using the composition in high-gloss electrosilvering coating, the prepared high-gloss electrosilvering coating composition is matched with black primer and varnish for use, the 20-degree gloss of a composite coating is more than 230, the glossiness of the composite coating is far higher than that of the conventional electrosilvering coating composition by 20 degrees and is within a range of 170-180, the water resistance and the recoating performance are qualified, and the composition can be matched with liquid varnish or varnish powder for use and is suitable for coating hubs.
In one example, the particle size of the aluminum powder in the silver electroplating aluminum paste is 8-14 μm, and the non-volatile content of the silver electroplating aluminum paste is 9.90-10.10%. The silver-electroplating aluminum paste suitable for the embodiment includes, but is not limited to, TS-408PM, which is available from Zhaoqing eastern ocean, and the aluminum powder has a particle size of 8 μm and a non-volatile content of 10.0%, or is selected from
Figure BDA0003124558440000032
A-41014, available from ECKART, had an aluminum powder particle size of 14 μm and a nonvolatile content of 10.0%.
In one example, the silver electroplating resin has a nonvolatile content of 7.5 to 8.5% and a Gardner viscosity of W to Z3. Suitable electro-silvering resins for use in this embodiment include, but are not limited to, resins selected from AMORSO-789A, available from huai' an research chemical company, inc, having a nonvolatile content of 8.5% and a gardner viscosity of Y-Z3, or resins selected from a-108, available from guangzhou boya chemical company, having a nonvolatile content of 8% and a gardner viscosity of W-Z.
In the present embodiment, the applicant found that the silver electroplating resin itself has almost no reactive group, and if the crosslinked cured resin is blended with the silver electroplating resin, the paint film can be endowed with good interlayer adhesion, water resistance and recoatability. However, the type and amount of the cross-linked resin blend interferes with the alignment of the silver electroplated aluminum powder, thereby reducing the gloss of the silver electroplated coating, such as a conventional acrylic resin + amino resin combination, or a polyester resin + amino resin combination. Therefore, the key of the formula design of the high-gloss electrosilvering coating is to select the cross-linked mixed resin with small interference on the arrangement of the electrosilvering aluminum powder and reduce the dosage of the cross-linked mixed resin on the premise of ensuring the performance of the coating. The applicant proves through experiments that: the blocked isocyanate resin has smaller interference on the arrangement of the silver-electroplating aluminum powder than the acrylic resin or polyester resin commonly used in the conventional silver-electroplating coating; the hydroxyl hyperbranched resin has the advantages of small molecular weight and large number of reaction functional groups, the hydroxyl hyperbranched resin can provide enough reaction group number on the premise of ensuring less blending resin consumption, and the blocked isocyanate resin and the hydroxyl hyperbranched resin react to form an elastic urethane bond, so that the brittleness of the high-molecular silver electroplating resin on a silver electroplating layer paint film is balanced, the silver electroplating coating has excellent flexibility, the requirement of recoatability of a composite coating is met, and the matching of the silver electroplating coating and powder varnish needing high-temperature baking and curing is realized.
In the present embodiment, the hydroxyl hyperbranched resin is polyester polyol and has a hyperbranched structure. In a preferred example, the hydroxyl hyperbranched resin has a non-volatile content of 53.0-63.0%, a viscosity of 150-550mPa.s @25 ℃, and a hydroxyl content of 4.8-6.3% calculated on the solid resin. The hydroxyl hyperbranched resin suitable for the invention includes, but is not limited to, CYGLAZ BB 500, a commercially available free-standing coating (china) limited having a non-volatile content of 53.0-55.0%, a viscosity of 150-250mpa.s @25 ℃, a hydroxyl content of 6.3% as a solid resin, or CYGLAZ BB 600, a similarly commercially available free-standing coating (china) limited having a non-volatile content of 61.0-63.0%, a viscosity of 400-550mpa.s @25 ℃, a hydroxyl content of 6.3% as a solid resin.
In the scheme, the existence of the blocked isocyanate simultaneously has good effect on improving the recoating adhesive force of the electrosilvering coating. In a preferred embodiment, the blocked isocyanate resin has a non-volatile content of 73.0 to 77.0%, a deblocking temperature of 110 to 150 ℃, and a blocked isocyanate functional group content of 8% to 12% by weight in the blocked isocyanate resin. The blocked isocyanate resin includes, but is not limited to, a blocked isocyanate resin selected from DESMODUR BL 3575SN, available from BAYER corporation, having a non-volatile content of 73.0 to 77.0%, a deblocking temperature of 112 ℃, a blocked isocyanate functional group content of 11.1% by weight in the blocked isocyanate resin, or a blocked isocyanate functional group selected from TKA-B75S, available from Asahi Chemicals corporation, having a non-volatile content of 73.0 to 77.0%, a deblocking temperature of 142 ℃, a blocked isocyanate functional group content of 11.2% by weight in the blocked isocyanate resin.
The existence of the anti-dropping silver additive is helpful for improving the recoating adhesion of the electro-silvering coating. In a preferred example, the silver drop prevention aid is a low acid modified polyester compound having a non-volatile content of 78.0 to 82%, such as silver drop prevention aid 120 available from proud chemical ltd.
In a preferred example, the auxiliary agent is selected from one or more of a leveling agent, an ultraviolet absorber, a light stabilizer, a coupling agent or a wetting and dispersing agent.
Further, the leveling agent is an acrylic leveling agent, including but not limited to, selected from DYNAADF-1, available from DYNEA corporation; the ultraviolet light absorber is selected from TINUVIN-384-2, available from BASF corporation, or CHISORB5228, available from Dibixi chemical trade (Shanghai) Co., ltd.; the light stabilizer is selected from TINUVIN-292, available from BASF corporation, or CHISORB532, available from Dibipy chemical trade (Shanghai) Co., ltd; the coupling agent was selected from SE 01-A2, available from shin-Etsu chemical Co.
Further, the auxiliary agent comprises the following components in percentage by weight based on the total weight of the high-gloss electrosilvering coating:
Figure BDA0003124558440000041
in a preferred example, the solvent is selected from one or more of ketone solvents, ester solvents and aromatic hydrocarbon solvents. Wherein the ester solvent is selected from one or more of propylene glycol methyl ether acetate, 3-ethoxy ethyl propionate, butyl acetate and ethyl acetate, and the ester solvent accounts for 66.0-70.0% of the total weight of the electrosilvering coating composition; the ketone solvent is selected from one or more of cyclohexanone, methyl amyl ketone, methyl isoamyl ketone and methyl isobutyl ketone, and the ketone solvent accounts for 16.0 to 20.0 percent of the total weight of the electrosilvering coating composition; the aromatic hydrocarbon solvent is selected from one or more of dimethylbenzene, S-100#, S-150#, and the aromatic hydrocarbon solvent accounts for 14.0-18.0% of the total weight of the electrosilvering coating composition.
Still another embodiment of the present invention provides a high-gloss electro-silvering paint whose raw material includes a high-gloss electro-silvering paint composition as described in the first embodiment above.
It can be understood that, since the raw material includes the electro-silver plating coating composition as described above, the electro-silver plating coating also has the effects brought by the electro-silver plating coating composition. Namely, the silver electroplating coating composition is matched with black primer and varnish for use, the 20-degree gloss of the composite coating is more than 230, the gloss of the composite coating is far higher than the 20-degree gloss of the conventional silver electroplating coating composition and is within the range of 170-180, the water resistance and the recoating performance are qualified, and the silver electroplating coating composition can be matched with liquid varnish or powder varnish for use and is suitable for coating automobile hubs.
Yet another embodiment of the present invention provides a method for preparing the above-mentioned electroplated silver paint, which comprises the steps of:
1) Passivating the silver-electroplating aluminum paste to obtain passivated silver-electroplating aluminum paste;
2) Dissolving hydroxyl hyperbranched resin and blocked isocyanate resin in a part of solvent, and uniformly mixing to obtain a mixed resin semi-finished product;
3) And uniformly mixing the silver electroplating resin and the passivated silver electroplating aluminum paste, mixing the mixture with the semi-finished product of the mixed resin, and adding the auxiliary agent and the residual solvent to obtain the high-gloss silver electroplating coating.
In some examples, step 1), the electro-silvered aluminum paste is passivated with a coupling agent. After the passivated electro-silvered aluminum paste is used in the preparation of the electro-silvered coating, the electro-silvered coating has better water resistance.
In other examples, in step 3), the silver electroplating resin is dispersed and dissolved in the ketone solvent and then mixed with the passivated silver electroplating aluminum paste. At the moment, the silver electroplating resin has better miscibility with other resins, and the obtained coating has strong adhesive force. In some preferred examples, the method for preparing the electro-silvering paint comprises the following steps:
1) Passivating the electroplated silver aluminum paste: putting the silver-electroplating aluminum paste and part of ester solvent into a container A, stirring at 300-400r/min, adding the coupling agent in a formula amount, stirring for 10-15min, then adding the silver-dropping-preventing auxiliary agent in a formula amount, continuously stirring for 30-40min, stopping stirring, taking part of ester solvent to flush the stirring paddle and the aluminum paste on the container wall, sealing the container A, and standing for 4h to passivate the aluminum paste for later use;
2) Preparing a mixed resin semi-finished product: putting part of ester solvent into a container B, stirring at 200-300r/min, putting the hydroxyl hyperbranched resin according to the formula amount, washing the container wall and a stirring paddle by using part of ester solvent, stirring for 5-10min, putting the blocked isocyanate according to the formula amount, increasing the stirring speed to 400-500r/min, continuing stirring for 20-30min, and stopping stirring for later use;
3) Another container C is found, the ketone solvent with the formula amount is added, the stirring is carried out under the condition of 200-300r/min, the silver electroplating resin with the formula amount is added, the stirring rotating speed is increased to 400-500r/min, the stirring is carried out for 5-10min, the silver electroplating aluminum paste in the step 1 is added, the residual ester solvent is taken out, the container A is washed and then added together, and the stirring is carried out for 20-30min;
4) Putting the semi-finished product of the mixed resin in the step 2 into a container C, washing the container B with a part of ester solvent, putting the mixture together, and stirring for 10-20min;
5) And (3) continuously adding the formula amount of the auxiliary agent, the residual ester solvent and the aromatic hydrocarbon solvent into the container C for one time, and continuously stirring for 30-40min to obtain the high-gloss electrosilvering coating composition.
In the preparation method, the high molecular weight electrosilvering resin with the ketone solvent has good dissolving power, and the electrosilvering resin is dissolved and dispersed by the ketone solvent, so that good miscibility between the electrosilvering resin and the blended crosslinking resin can be ensured; the adoption of part of aromatic hydrocarbon solvents can avoid biting and biting of the priming paint during wet-on-wet spraying of the electrosilvering coating and the black priming paint.
Another embodiment of the present invention provides the use of the high gloss electro-silvering paint as described above in the painting of automobile wheel hubs.
Specifically, the high-gloss electrosilvering coating is used for coating automobile aluminum alloy hubs.
The technical solution of the present invention is described below with reference to some specific examples:
raw materials:
electroplated silver-aluminum paste TS-408PM, purchased from Zhaoqing eastern ocean, or
Figure BDA0003124558440000062
A-41014, available from ECKART corporation;
the electroplated silver resin AMORSO-789A is purchased from Huaian Shanghai chemical industry Co., ltd, or A-108 is purchased from Guangzhou Baiya chemical industry Co., ltd;
hydroxyl hyperbranched resin CYGLAZ BB 500, available from coatings from libanor (china) ltd, or CYGLAZ BB 600, also available from coatings from libanor (china) ltd;
blocked isocyanate resin DESMODUR BL 3575SN from BAYER, or TKA-B75S from Asahi Chemicals;
the silver drop prevention auxiliary agent 120 is purchased from Aoyan chemical Co., ltd, shanghai;
acrylic leveling agent DYNAODD F-1, available from DYNEA corporation;
the UV absorber TINUVIN-384-2, available from BASF corporation, or selected from CHISORB5228, available from Dibipy chemical trade (Shanghai) Co., ltd;
light stabilizer TINUVIN-292, available from BASF corporation, or CHISORB532, available from Dibixi chemical trade (Shanghai) Co., ltd;
coupling agent SE 01-A2, available from shin-Etsu chemical Co.
Example 1
The raw material composition formula of the high-gloss electrosilvering coating is shown in table 1.
Table 1 example 1 parts by weight of raw materials
Figure BDA0003124558440000061
Figure BDA0003124558440000071
The preparation method of the high-gloss electrosilvering coating comprises the following steps:
1) Passivating the electroplated silver aluminum paste: putting 2 parts of silver-electroplated aluminum paste and 10 parts of butyl acetate into a container A, stirring at 300-400r/min, putting 0.02 part of coupling agent SE 01-A2, stirring for 10-15min, then putting 0.04 part of silver-dropping-preventing auxiliary agent 120, continuing stirring for 30-40min, stopping stirring, washing the stirring paddle and the aluminum paste on the wall of the container with 8.89 parts of butyl acetate solvent, sealing the container A, and standing for 4h to passivate the aluminum paste for later use;
2) Preparing a mixed resin semi-finished product: putting 5 parts of propylene glycol methyl ether acetate into a container B, stirring at 200-300r/min, putting 0.06 part of hydroxyl hyperbranched resin CYGLAZ BB 500, washing the container wall and a stirring paddle by 2 parts of propylene glycol methyl ether acetate, stirring for 5-10min, then putting 0.4 part of blocked isocyanate DESMODUR BL 3575SN, increasing the stirring speed to 400-500r/min, continuing stirring for 20-30min, and stopping stirring for later use;
3) Another container C is searched, 18 parts of methyl isobutyl ketone is added, stirring is carried out under the condition of 200-300r/min, 5.0 parts of silver electroplating resin AMORSO-789A is added, the stirring rotating speed is increased to 400-500r/min, stirring is carried out for 5-10min, the silver electroplating aluminum paste in the step 1 is added, 10 parts of propylene glycol methyl ether acetate are taken to wash the container A and then are added together, and stirring is carried out for 20-30min;
4) Putting the semi-finished product of the mixed resin in the step 2 into a container C, washing the container B with 10 parts of propylene glycol methyl ether acetate, putting the washed container B together, and stirring for 10-20min;
5) And (3) continuously adding the formula amount auxiliary agent, the rest 9 parts of propylene glycol methyl ether acetate, 3.5 parts of ethyl 3-ethoxypropionate and 16 parts of aromatic solvent S-100# in the container C for one time, and continuously stirring for 30-40min to obtain the high-gloss electrosilvering coating composition.
Comparative example 1
Example 1 was repeated, with the difference that the hydroxy hyperbranched resin of example 1 was replaced by commercially available hydroxy acrylic resin AP 545 and the like in terms of solid content, and the amount of other materials was unchanged.
Comparative example 2
Example 1 was repeated except that the blocked isocyanate resin of example 1 was replaced with a commercially available amino resin, BR20SE and the like, in terms of solid content, and the other materials were used in the same amounts.
Comparative example 3
Example 1 was repeated, except that the blocked isocyanate resin DESMODUR BL 3575SN and the hydroxy hyperbranched resin CYGLAZ BB 500 of example 1 were replaced by commercially available thermosetting acrylic resins TAR-3753-70 and amino resin BR20SE, etc., in the solid amounts, and the solid ratio of TAR-3753-70 and BR20SE was 7.
Comparative example 4
Example 1 was repeated with the difference that the blocked isocyanate resin DESMODUR BL 3575SN and the hydroxy hyperbranched resin CYGLAZ BB 500 of example 1 were replaced by commercially available polyester resin SETAL173 VS 60 and amino resin BR20SE with the same solids content, the solids ratio of SETAL173 VS 60 and BR20SE was 7.
Comparative example 5
Comparative example 3 is a commercially available general electro-silvering paint having an electro-silvering aluminum paste content of 0.19% by solid, substantially equivalent to example 1.
Comparative example 6
Example 1 was repeated except that comparative example 6 had the following parts by weight of the raw materials as shown in table 2.
Table 2 example 6 parts by weight of starting materials
Figure BDA0003124558440000081
Comparative example 7
Example 1 was repeated except that comparative example 7 contained the following parts by weight of the starting materials as shown in Table 3.
Table 3 comparative example 7 parts by weight of raw materials
Figure BDA0003124558440000082
Comparative example 8
Example 1 was repeated except that the parts by weight of the feed of comparative example 8 were as indicated in Table 4, and the parts by weight of the feed of comparative example 8
Figure BDA0003124558440000091
Comparative example 9
Example 1 was repeated except that the parts by weight of the starting materials of comparative example 9 are as shown in Table 5, table 5 and comparative example 9
Figure BDA0003124558440000092
Test example 1 high gloss electro-silvering paint Performance test
a. Preparation of composite coating sample matched with liquid varnish
Substrate: aluminum alloy sheet coated with powder primer
A degraded coating composition: aluminum alloy sheet coated with powder primer + black primer (140 ℃ 25min bake) + silver plating coating + liquid varnish (140 ℃ 25min bake)
Recoating 1 defective coating composition: a defective coating sample plate + black primer (140 ℃ 25min bake) + electro-silvering coating + liquid varnish (140 ℃ 25min bake)
Recoating 2 defective coating composition: repainting 1 defective coating sample plate + black primer (140 ℃ 25min bake) + electro-silvering coating + liquid varnish (140 ℃ 25min bake)
b. Preparation of composite coating sample plate matched with powder varnish
Substrate: aluminum alloy sheet coated with powder primer
A degraded coating composition: aluminum alloy panels coated with powder primer + black primer (80 ℃ C. 5min flash dried) + electro-silvered coating (140 ℃ C. 25min bake) + powder clear coat (180 ℃ C. 20min bake)
Recoating 1 defective coating composition: a sample of defective coating plus black primer (80 ℃ C. 5min flash dried) + silver plating coating (140 ℃ C. 25min bake) + powder varnish (180 ℃ C. 20min bake)
Recoating 2 defective coating composition: recoat 1. Degraded product coating template + black primer (80 ℃ C. 5min flash dried) + electro-silvered paint (140 ℃ C. 25min baked) + powder varnish (180 ℃ C. 20min baked)
The test methods for the properties are shown in Table 6:
TABLE 6 Performance test method
Detecting items Detection method and requirements
Appearance of coating film Visual inspection shows that the paint film is flat and the aluminum powder is arranged flatly
20 degree gloss ≥230
Adhesion force Adhesion force less than or equal to 1 grade, 2mm lattice method
Water resistance At 40 deg.C for 240 hr, no bubble, no white peeling, and secondary adhesion not more than 1 grade
2-time recoatability Adhesion force less than or equal to 1 grade, 2mm lattice method
CASS (acid salt spray resistance) 240h, maximum unilateral corrosion less than or equal to 3mm
The baking varnish performances of example 1 and comparative examples 1 to 7 were tested by the above-mentioned methods, and the results are shown in tables 7, 8, 9, 10, 11 and 12.
TABLE 7 film properties associated with liquid varnishes of example 1 and comparative examples 1 to 3
Figure BDA0003124558440000101
TABLE 8 film properties associated with powder varnishes of example 1 and comparative examples 1 to 3
Figure BDA0003124558440000102
Figure BDA0003124558440000111
TABLE 9 film Properties associated with liquid varnishes of comparative examples 4 to 7
Figure BDA0003124558440000112
TABLE 10 film properties associated with powder varnishes of comparative examples 4 to 7
Figure BDA0003124558440000113
TABLE 11 film properties matched with liquid varnishes of comparative examples 8 to 9
Figure BDA0003124558440000114
TABLE 12 film properties associated with powder varnishes of comparative examples 8 to 9
Figure BDA0003124558440000115
Figure BDA0003124558440000121
As can be seen from tables 7 and 8, the high-gloss electrosilvering coating prepared in example 1 is matched with liquid varnish and powder varnish, the 20-degree gloss of the composite coating is more than 230, and the coating film is qualified in water resistance, recoat and other properties.
Comparative example 1 the hydroxyl hyperbranched resin in example 1 was replaced by a commercially available hydroxyl acrylic resin AP 545 and the like, which had a small amount of hydroxyl acrylic resin and thus had less interference with the aluminum powder alignment, and the composite coating had a 20 ° gloss of > 230 and a gloss of acceptable gloss, but the hydroxyl acrylic resin had an insufficient number of reactive groups, resulting in insufficient crosslinking density with the blocked isocyanate resin and unacceptable water, recoat and acid resistance.
Comparative example 2 the blocked isocyanate resin of example 1 was replaced with commercially available amino resin BR20SE and the like at a solids level, the amino resin BR20SE interfered with the aluminum powder alignment, the silver electroplated composite coating had a 20 ° gloss of < 230 and a gloss that was not acceptable, and the amino resin reacted with the hydroxyl hyperbranched resin to give a crosslink density that was not as high as the crosslink density produced by the reaction of the blocked isocyanate resin with the hydroxyl hyperbranched resin, resulting in unacceptable water, recoat and acid resistance to salt spray.
Comparative example 3 the solid content of commercial thermosetting acrylic resin TAR-3753-70 and amino resin BR20SE and the like is used for replacing the blocked isocyanate resin DESMODUR BL 3575SN and the hydroxyl hyperbranched resin CYGLAZ BB 500 in the example 1, the acrylic resin and the amino resin are fully crosslinked, the water resistance, recoating and acid salt mist resistance of the coating film are qualified, but the arrangement of the silver-electroplated aluminum powder is interfered, the 20-degree gloss of the silver-electroplated composite coating is less than 230, and the gloss is unqualified.
As can be seen from tables 9 and 10, in comparative example 4, the blocked isocyanate resin DESMODUR BL 3575SN and the hydroxyl hyperbranched resin CYGLAZ BB 500 in example 1 were replaced by the commercial solid contents of polyester resin SETAL173 VS 60 and amino resin BR20SE, the polyester resin and the amino resin were crosslinked sufficiently, the coating film was water-resistant, recoated and acid-resistant, but the arrangement of the silver-electroplated aluminum powder was disturbed, and the 20 ° gloss of the silver-electroplated composite coating was less than 230, and the gloss was not qualified.
Comparative example 5 is a commercial conventional electro-silvered paint, the electro-silvered composite coating has a 20 ℃ gloss of less than 230 and a non-qualified gloss.
In comparative example 6, the dosage of the silver electroplating resin AMORSO-789A is higher than the upper limit value of the range of 6 percent, the 20-degree gloss of the composite coating is more than 230, and the gloss is qualified, but the dosage of the silver electroplating resin is too much, the coating film of the silver electroplating layer becomes brittle, and the performances of the composite coating such as water resistance, recoating and the like are unqualified.
Comparative example 7, the use level of the silver electroplating resin AMORSO-789A is lower than the lower limit value of the range of 4%, the arrangement of the silver electroplating aluminum powder is poor, the 20-degree gloss of the silver electroplating composite coating is less than 230, and the gloss is unqualified.
As can be seen from tables 11 and 12, in comparative example 8, the dosage of the hydroxyl hyperbranched resin CYGLAZ BB 500 is lower than the lower limit value of the range of 0.04%, the 20-degree gloss of the composite coating is more than 230, and the gloss is qualified, but the reduction of the number of the hydroxyl reactive groups causes insufficient crosslinking density of a paint film of the electrosilvering layer, and the performances of the paint film, such as water resistance, recoating performance, acid resistance, salt mist resistance and the like, are unqualified.
In comparative example 9, the use level of the blocked isocyanate resin DESMODUR BL 3575SN is lower than the lower limit value of the range of 0.3 percent, the 20-degree gloss of the composite coating is more than 230, and the gloss is qualified, but the reduction of the number of the isocyanate reaction groups causes the crosslinking density of the paint film of the silver electroplating layer to be insufficient, and the performances of the paint film such as water resistance, recoating resistance, acid resistance and the like are unqualified.
Example 2
Example 1 was repeated except that in example 2, the raw materials were used in the amounts shown in Table 13.
TABLE 13 example 2 parts by weight of starting materials
Figure BDA0003124558440000131
Example 3
Example 1 was repeated except that example 3 had the following weight parts of the starting materials as shown in Table 14. Wherein the blocked isocyanate resin is TKA-B75S, and the non-volatile content is 75%.
TABLE 14 example 3 parts by weight of starting materials
Figure BDA0003124558440000132
The preparation method of the high-gloss electrosilvering coating comprises the following steps:
1) Passivating the electroplated silver aluminum paste: putting 2 parts of silver-electroplated aluminum paste and 10 parts of butyl acetate into a container A, stirring at 300-400r/min, putting 0.02 part of coupling agent SE 01-A2, stirring for 10-15min, then putting 0.04 part of silver-dropping-preventing auxiliary agent 120, continuing stirring for 30-40min, stopping stirring, washing the stirring paddle and the aluminum paste on the wall of the container with 8.99 parts of butyl acetate solvent, sealing the container A, and standing for 4h to passivate the aluminum paste for later use;
2) Preparing a mixed resin semi-finished product: putting 5 parts of propylene glycol methyl ether acetate into a container B, stirring at 200-300r/min, putting 0.06 part of hydroxyl hyperbranched resin CYGLAZ BB 500, washing the container wall and a stirring paddle by 2 parts of propylene glycol methyl ether acetate, stirring for 5-10min, then putting 0.4 part of blocked isocyanate TKA-B75S, increasing the stirring speed to 400-500r/min, continuing stirring for 20-30min, and stopping stirring for later use;
3) Another container C is searched, 18 parts of methyl isobutyl ketone is added, stirring is carried out under the condition of 200-300r/min, 5.0 parts of silver electroplating resin AMORSO-789A is added, the stirring rotating speed is increased to 400-500r/min, stirring is carried out for 5-10min, the silver electroplating aluminum paste in the step 1 is added, 10 parts of propylene glycol methyl ether acetate are taken to wash the container A and then are added together, and stirring is carried out for 20-30min;
4) Putting the semi-finished product of the mixed resin obtained in the step (2) into a container C, washing the container B with 10 parts of propylene glycol monomethyl ether acetate, putting the washed container B together, and stirring for 10-20min;
5) And (3) continuously adding the formula amount auxiliary agent, the rest 9 parts of propylene glycol methyl ether acetate, 3.5 parts of ethyl 3-ethoxypropionate and 16 parts of aromatic solvent S-100# in the container C for one time, and continuously stirring for 30-40min to obtain the high-gloss electrosilvering coating composition.
Example 4
Example 4 the raw material parts by weight of the high gloss electro-silvered coating composition are shown in table 15.
TABLE 15 example 4 parts by weight of starting materials
Figure BDA0003124558440000141
The preparation method of the high-gloss electrosilvering coating comprises the following steps:
1) Passivating the electroplated silver aluminum paste: putting 2 parts of silver-electroplated aluminum paste and 10 parts of butyl acetate into a container A, stirring at 300-400r/min, putting 0.02 part of coupling agent SE 01-A2, stirring for 10-15min, then putting 0.04 part of silver-dropping-preventing auxiliary agent 120, continuing stirring for 30-40min, stopping stirring, washing the stirring paddle and the aluminum paste on the wall of the container with 7.88 parts of butyl acetate solvent, sealing the container A, and standing for 4h to passivate the aluminum paste for later use;
2) Preparing a mixed resin semi-finished product: putting 5 parts of propylene glycol methyl ether acetate into a container B, stirring at 200-300r/min, putting 0.06 part of hydroxyl hyperbranched resin CYGLAZ BB 500, washing the container wall and a stirring paddle by 2 parts of propylene glycol methyl ether acetate, stirring for 5-10min, putting 0.4 part of blocked isocyanate DESMODUR BL 3575SN, increasing the stirring speed to 400-500r/min, continuing stirring for 20-30min, and stopping stirring for later use;
3) Another container C is found, 18 parts of methyl isobutyl ketone is added, stirring is carried out under the condition of 200-300r/min, 5.0 parts of silver electroplating resin AMORSO-789A is added, the stirring rotating speed is increased to 400-500r/min, stirring is carried out for 5-10min, the silver electroplating aluminum paste in the step 1 is added, 10 parts of propylene glycol methyl ether acetate is taken to wash the container A and then is added together, and stirring is carried out for 20-30min;
4) Putting the semi-finished product of the mixed resin in the step 2 into a container C, washing the container B with 10 parts of propylene glycol methyl ether acetate, putting the washed container B together, and stirring for 10-20min;
5) And (3) continuously adding the formula amount auxiliary agent, the remaining 9 parts of propylene glycol monomethyl ether acetate, 3.5 parts of ethyl 3-ethoxypropionate and 16 parts of aromatic solvent S-100# into the container C for one time, and continuously stirring for 30-40min to obtain the high-gloss electrosilvering coating composition.
Example 5
The hyperbranched resin is the same as the hyperbranched resin in example 1, except that the hydroxyl hyperbranched resin is CYGLAZ BB 600, and the total amount of the hydroxyl hyperbranched resin in the formula is 0.04%.
Example 6
The difference from example 1 is that the silver-aluminum electroplating slurry is
Figure BDA0003124558440000151
A-41014, the aluminum powder particle size is 14 μm, the non-volatile content is 10.0%.
Example 7
The same as example 1 except that the blocked isocyanate resin was TKA-B75S having a nonvolatile content of 75%.
Example 8
The same as example 1 except that the silver plating resin was A-108, and the nonvolatile content thereof was 8%.
Example 9
The difference from example 1 is that the silver plating resin accounts for 4wt%, the hydroxyl hyperbranched resin accounts for 0.04wt%, and the blocked isocyanate resin accounts for 0.3wt%.
Example 10
The difference from example 1 is that the silver plating resin accounts for 6wt% of the total amount, the hydroxyl hyperbranched resin accounts for 0.06wt% of the total amount, and the blocked isocyanate resin accounts for 0.5wt% of the total amount.
The high gloss electrosilvering coating compositions obtained in examples 2 to 10 were tested for gloss and main coating properties in the manner of test example 1 described above, and the test results are shown in tables 16 and 17, which are similar to those of example 1.
TABLE 16 Primary coating Properties of the high gloss electrosilvered coatings of examples 2-10, in combination with liquid varnishes
Examples Gloss of Water resistance Recoatability CASS
Example 2 236, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 3 233, passed Grade 0, pass Grade 0, pass 3mm, qualified
Example 4 241, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 5 238, qualification of Grade 0, pass Grade 0, pass 2mm, qualified
Example 6 235, qualified Grade 0, pass Grade 0, pass 3mm, qualified
Example 7 234, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 8 233, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 9 236, qualified Grade 0, pass Grade 0, pass 3mm, qualified
Example 10 239, qualified Grade 0, pass Grade 0, pass 1mm, qualified
TABLE 17 Primary coating Properties of high gloss electrosilvering coatings of examples 2-10 in combination with powder varnishes
Examples Gloss (E) Water resistance Recoatability CASS
Example 2 234, qualified Grade 0, pass Grade 0, pass 1mm, qualified
Example 3 235, qualified Grade 0, pass Grade 1, qualified 3mm, qualified
Example 4 243, pass Grade 0, pass Grade 0, pass 2mm, qualified
Example 5 239, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 6 232, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 7 236, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 8 235, qualified Grade 0, pass Grade 0, pass 2mm, qualified
Example 9 238, qualification Grade 0, pass Grade 1, good 2mm, qualified
Example 10 241, qualified Grade 0, pass Grade 0, pass 1mm, qualified
Example 11
The same as example 1, except that the aluminum powder was not passivated with the coupling agent SE 01-A2, but directly charged in step 5, resulted in the high-gloss electro-silvered paint having unsatisfactory water resistance.
Example 12
The difference from example 1 is only that the solvent for dispersing the hydroxyl hyperbranched resin is an aromatic hydrocarbon solvent, and as a result, the obtained high-gloss electrosilvering coating has poor adhesion for recoating, which may be caused by the strong polarity of the hydroxyl hyperbranched resin, the hydroxyl hyperbranched resin is not uniformly dispersed in the nonpolar aromatic hydrocarbon solvent, agglomeration is generated, and finally, the hydroxyl hyperbranched resin cannot fully react with the blocked isocyanate resin, and the coating film is not fully crosslinked.
Example 13
The difference from example 1 was that only the silver electroplating resin was not dissolved and dispersed in advance with the ketone solvent, but the silver electroplating resin was charged into the vessel B after blocking the isocyanate resin in step 2), and as a result, the obtained silver electroplating coating composition had a 20 ℃ gloss of < 230 and an adhesion failure due to a large molecular weight of the silver electroplating resin which was not dissolved and dispersed in advance with the ketone solvent having a strong dissolving power, resulting in poor miscibility of the silver electroplating resin with other resins and a decrease in adhesion.
Example 14
The only difference from example 1 is that the starting materials used in example 14 are shown in Table 18. The film performance test result of the high-gloss electro-silvering coating composition prepared in example 14 is similar to that of example 1.
TABLE 18 example 14 parts by weight of starting materials
Figure BDA0003124558440000171
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.

Claims (10)

1. A high-gloss electrosilvering coating composition is characterized by comprising the following components in percentage by weight:
Figure FDA0003124558430000011
2. the high-gloss electrosilvering coating composition as claimed in claim 1, wherein the particle size of the aluminum powder in the electrosilvering aluminum paste is 8-14 μm, and the non-volatile content of the electrosilvering aluminum paste is 9.90-10.10%.
3. The high gloss electrosilvering coating composition according to claim 1, wherein the electrosilvering resin has a nonvolatile content of 7.5-8.5% and a Gardner viscosity of W-Z3.
4. The high gloss electrosilvering coating composition according to claim 1, wherein the hydroxyl hyperbranched resin has a non-volatile content of 53.0-63.0%, a viscosity of 150-550mpa.s @25 ℃, and a hydroxyl content of 4.8-6.3% calculated on the solid resin.
5. The high gloss electrosilvering coating composition according to claim 1, wherein the blocked isocyanate resin has a nonvolatile content of 73.0-77.0%, a deblocking temperature of 110-150 ℃, and a blocked isocyanate functional group content of 8-12 wt% in the blocked isocyanate resin;
preferably, the silver drop-proof auxiliary agent is a low-acidity modified polyester compound, and the non-volatile content of the silver drop-proof auxiliary agent is 78.0-82%.
6. The high-gloss electrosilvering coating composition according to claim 1, wherein the auxiliary agent is one or more selected from leveling agents, ultraviolet absorbers, light stabilizers, coupling agents or wetting and dispersing agents;
preferably, the assistant comprises the following components in percentage by weight based on the total weight of the electrosilvering coating composition:
Figure FDA0003124558430000012
7. the high gloss electrosilvering coating composition according to claim 1, wherein the solvent is one or more selected from the group consisting of ketone solvents, ester solvents and aromatic hydrocarbon solvents;
preferably, the ester solvent is selected from one or more of propylene glycol methyl ether acetate, ethyl 3-ethoxypropionate, butyl propionate, butyl acetate and ethyl acetate, and the ester solvent accounts for 56.0-60.0% of the total weight of the electrosilvering coating composition;
preferably, the ketone solvent is selected from one or more of cyclohexanone, methyl amyl ketone, methyl isoamyl ketone and methyl isobutyl ketone, and the ketone solvent accounts for 16.0-20.0% of the total weight of the electrosilvering coating composition;
preferably, the aromatic hydrocarbon solvent is selected from one or more of xylene, S-100#, S-150#, and the aromatic hydrocarbon solvent accounts for 14.0-18.0% of the total weight of the electrosilvering coating composition.
8. A high gloss electro-silvering paint, characterized in that the raw material of the electro-silvering paint comprises the high gloss electro-silvering paint composition as claimed in any one of claims 1 to 7.
9. The method for preparing high-gloss electrosilvering paint according to claim 8, comprising the steps of:
1) Passivating the electroplated silver aluminum paste to obtain passivated electroplated silver aluminum paste;
2) Dissolving hydroxyl hyperbranched resin and blocked isocyanate resin in a part of solvent, and uniformly mixing to obtain a mixed resin semi-finished product;
3) And uniformly mixing the silver electroplating resin and the passivated silver electroplating aluminum paste, mixing the mixture with the semi-finished product of the mixed resin, and adding the auxiliary agent and the residual solvent to obtain the high-gloss silver electroplating coating.
10. The use of the high gloss electro-silvering paint according to claim 8 in the painting of automobile hubs.
CN202110685784.6A 2021-06-21 2021-06-21 High-gloss electrosilvering coating composition, electrosilvering coating and preparation method thereof Pending CN115572545A (en)

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