CN111548667A - Composite polysiloxane protective finish paint for PVD (physical vapor deposition) and preparation method thereof - Google Patents
Composite polysiloxane protective finish paint for PVD (physical vapor deposition) and preparation method thereof Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
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- C09D5/08—Anti-corrosive paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4419—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications with polymers obtained otherwise than by polymerisation reactions only involving carbon-to-carbon unsaturated bonds
- C09D5/443—Polyepoxides
- C09D5/4457—Polyepoxides containing special additives, e.g. pigments, polymeric particles
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/4473—Mixture of polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
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Abstract
The invention belongs to the technical field of coating and coating protection, and provides a composite polysiloxane protective finish paint for PVD (physical vapor deposition) and a preparation method thereof, wherein the composite polysiloxane protective finish paint is prepared by a silane coupling agent, an organic metal precursor, a composite polymer resin, an ultraviolet absorbent and the like after hydrolysis and polycondensation reaction under the action of an acid catalyst, and the specific formula comprises the following components in percentage by weight: the invention relates to a polysiloxane PVD protective finish paint, which is prepared by reacting a silane coupling agent, an organic metal precursor, polymer resin, an ultraviolet absorbent, an organic solvent and water.
Description
Technical Field
The invention relates to a composite polysiloxane protective finish paint for PVD (physical vapor deposition) and a preparation method thereof, belonging to the technical field of coating and coating protection.
Background
PVD is an ion plating technology, has the characteristics of high deposition speed, low processing temperature, compact and uniform film layer, strong adhesive force, good platability, wide platable materials and the like, is continuously and widely applied to processing of automobile parts, is green and environment-friendly compared with the traditional water electroplating, and better meets the requirements of intelligent manufacturing and sustainable development. The PVD carries out surface metallization processing on automobile parts, generally adopts a structure of 'base material + priming paint + PVD metal coating + finishing paint', the base material is PC, ABS or PC/ABS and the like, the priming paint is used for reducing the surface roughness of the base material and improving the adhesive force of the PVD metal layer, the PVD metal layer is plated with Al, In, Cr and the like and is used for providing decorative effects such as high light, mirror surface and the like or functions such as light transmission, wave transmission and the like, the finishing paint is a transparent protective layer, the PVD protective finish paint has decisive effect on PVD corrosion resistance, weather resistance, hardness, wear resistance and other physical properties, the current PVD protective finish paint has two preparation methods, one is that a SiOx (x is 1, 2) film layer is deposited in situ when a PVD vacuum metal plating layer is plated, the film layer has wide visible region transparency, has little influence on the reflectivity of visible light, and has strong mechanical property and chemical stability, but the method has high requirement on equipment and is easy to cause metal target poisoning; the other method is to coat polyacrylate or polyurethane protective coating on the surface of the PVD metal coating, the method is simple to operate, and has low requirements on equipment, but when the two coatings are applied to the PVD of the automobile exterior trimming parts, the comprehensive properties are insufficient, such as poor adhesion, low hardness, poor weather resistance, weak metal corrosion protection effect and the like.
Disclosure of Invention
The invention provides a composite polysiloxane protective finish paint for PVD (physical vapor deposition) and a preparation method thereof, which are used for the surface of a PVD metal coating and have the advantages of good adhesive force, high hardness, corrosion resistance and excellent aging resistance.
In order to realize the aim, the technical scheme of the invention is as follows: a composite polysiloxane protective finish paint for PVD is characterized in that the finish paint is prepared by a silane coupling agent, an organic metal precursor, a composite polymer resin, an ultraviolet absorbent and the like after hydrolysis and polycondensation reaction under the action of an acid catalyst, and the specific formula is as follows (in percentage by weight):
in the composite polysiloxane protective finishing paint for PVD, the silane coupling agent is ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane, n-hexyltrimethoxysilane, n-hexyltriethoxysilane, n-octyltrimethoxysilane, n-octyltriethoxysilane, n-decyltrimethoxysilane, n-decyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (2, 3-glycidoxy) propyltriethoxysilane, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, n-decyltrimethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, 3- (methacryloyloxy) propyl trimethoxy silane, 3- (methacryloyloxy) propyl triethoxy silane, phenyl trimethoxy silane, phenyl triethoxy silane, 3-mercaptopropyl trimethoxy silane, 3-mercaptopropyl triethoxy silane, 1, 2-bis (trimethoxy silicon) ethane and bis- [3- (triethoxy silicon) propyl ] -tetrasulfide.
In the composite polysiloxane protective finishing paint for PVD, the silane coupling agent is preferably a plurality of compounds of ethyl orthosilicate, methyltrimethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, n-propyltrimethoxysilane, isobutyltrimethoxysilane, n-hexyltrimethoxysilane, n-octyltrimethoxysilane, n-decyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, phenyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane and 1, 2-bis (trimethoxy silicon) ethane.
In the composite polysiloxane protective finish paint for PVD, the silane coupling agent is a compound of a plurality of tetraethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, vinyl trimethoxysilane, isobutyl trimethoxysilane, 3- (2, 3-epoxypropoxy) propyl trimethoxysilane, 3- (methacryloyloxy) propyl trimethoxysilane and phenyl trimethoxysilane.
In the composite polysiloxane protective finish paint for PVD, the organic metal precursor is one of ethyl titanate, isopropyl titanate, n-butyl zirconate and aluminum isopropoxide, and preferably one of isopropyl titanate, n-butyl titanate and aluminum isopropoxide.
In the composite polysiloxane protective finishing paint for PVD, the polymer resin is one or more of amino resin, hyperbranched polyester resin, epoxy resin and polycarbonate diol, and preferably one or two of amino resin and epoxy resin.
In the composite polysiloxane protective finishing paint for PVD, the ultraviolet absorbent is nano TiO2, nano ZnO and nano CeO2 ethanol dispersion liquid, the solid content is 15-40%, and the particle size is 10-100 nm.
In the composite polysiloxane protective finish paint for PVD, the organic solvent is one or more of methanol, ethanol, isopropanol, n-butanol, 2-butanol, propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether, preferably one or more of ethanol, isopropanol and n-butanol, and the acid catalyst is one of hydrochloric acid, nitric acid, acetic acid and p-toluenesulfonic acid, preferably one of hydrochloric acid and acetic acid.
A preparation method of composite polysiloxane protective finish paint for PVD is characterized by comprising the following steps: adding a silane coupling agent and an organic solvent into a reaction bottle at room temperature, stirring for 10min, adding a mixed solution of an acid catalyst and water, heating to 30-60 ℃, reacting for 20-60 min, adding an organic metal precursor, continuing to react for 6-12 h, cooling to room temperature, adding a polymer resin and an ultraviolet absorbent, and continuing to stir for 2-5 h to obtain the composite polysiloxane protective finish paint for PVD.
In the composite polysiloxane protective finish paint for PVD, the curing temperature is 80-150 ℃, the curing time is 30-240 min, preferably the curing temperature is 100-130 ℃, the curing time is 45-150 min, and the thickness of a cured dry film is 1-10 mu m, preferably 3-8 mu m.
In the preparation and application method of the polysiloxane electrophoretic coating, the substrate PVD metal plating layer is aluminum, indium, chromium, and the like, preferably aluminum, and the film thickness, adhesion (cross cut), alkali resistance (pH 13.5), CASS, xenon lamp aging resistance, and the like of the substrate PVD metal plating layer are tested by using GMW 1699 standard.
Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes the polysiloxane generated by the reaction of the silane coupling agent as the PVD protective finish, is colorless and transparent, has good adhesive force on the surface of a metal coating, high hardness, strong scratch resistance and protective effect, and has the following beneficial effects compared with the prior art:
1. polysiloxane is used as film-forming resin, and the bond energy of the 'Si-O' bond is higher than that of the 'C-C' bond, so that the film-forming resin has stronger weather resistance and corrosion resistance than common polyacrylic resin, polyurethane finish and the like;
2. an organic metal precursor is introduced into the formula, and forms an M-O (M metal) bond after hydrolysis and polycondensation, and the performances of flexibility, corrosion resistance, aging resistance and the like of the polysiloxane can be obviously improved after the organic metal precursor is crosslinked with an Si-O bond;
3. the polymer resin material is introduced into the formula, and the resin contains active groups such as hydroxyl, amino, carboxyl or epoxy groups, and the like, and can react with 'Si-OH' in polysiloxane in the thermosetting process, so that the crosslinking density of the coating can be improved, and the curing temperature of the coating can be reduced;
4. the nano particle ultraviolet absorbent is also introduced into the formula, so that the aging resistance of the polysiloxane coating can be obviously enhanced.
Detailed Description
Example 1
A composite polysiloxane protective finish paint for PVD comprises the following formula (weight percentage):
the preparation and application method comprises the following steps:
adding ethyl orthosilicate, methyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propyl trimethoxysilane, ethanol and isopropanol into a reaction bottle at room temperature, stirring for 10min, adding an acetic acid catalyst and water mixed solution, heating to 30 ℃, reacting for 60min, adding butyl titanate, continuing to react for 12h, cooling to room temperature, adding amino resin and nano CeO2And (3) continuously stirring the ethanol dispersion liquid (with the solid content of 20 percent and the particle size of 20nm) for 2 hours to obtain the composite polysiloxane protective finish paint for PVD, coating the composite polysiloxane protective finish paint on the PVD aluminized surface, and curing for 150min at 100 ℃, wherein the film properties are shown in Table 1.
Example 2
A composite polysiloxane protective finish paint for PVD comprises the following formula (weight percentage):
the preparation and application method comprises the following steps:
adding ethyl orthosilicate, isobutyl trimethoxy silane, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol, isopropanol and n-butanol into a reaction bottle at room temperature,stirring for 10min, adding mixed solution of hydrochloric acid catalyst and water, heating to 60 deg.C, reacting for 20min, adding isopropyl titanate, reacting for 6 hr, cooling to room temperature, adding epoxy resin and nanometer TiO2And (3) continuously stirring the ethanol dispersion liquid (with the solid content of 15 percent and the particle size of 100nm) for 5 hours to obtain the composite polysiloxane protective finish paint for PVD, coating the composite polysiloxane protective finish paint on the PVD aluminized surface, and curing for 45min at 130 ℃, wherein the film properties are shown in Table 1.
Example 3
A composite polysiloxane protective finish paint for PVD comprises the following formula (weight percentage):
the preparation and application method comprises the following steps:
adding ethyl orthosilicate, methyltrimethoxysilane, isobutyltrimethoxysilane, phenyltrimethoxysilane, ethanol and n-butanol solvent into a reaction bottle at room temperature, stirring for 10min, adding an acetic acid catalyst and water mixed solution, heating to 35 ℃ to react for 30min, adding tetrabutyl titanate, continuously reacting for 8h, cooling to room temperature, adding amino resin and nano ZnO ethanol dispersion (solid content is 40%, particle size is 40nm), continuously stirring for 3h to obtain the composite polysiloxane protective finish paint for PVD, coating the composite polysiloxane protective finish paint on a PVD aluminized surface, and curing at 125 ℃ for 90min, wherein the film properties are shown in Table 1.
Example 4
A composite polysiloxane protective finish paint for PVD comprises the following formula (weight percentage):
the preparation and application method comprises the following steps:
at room temperature, adding ethyl orthosilicate, vinyl trimethoxy silane, dimethyl dimethoxy silane and 3- (2, 3-epoxy) into a reaction bottlePropoxy) propyl trimethoxy silane, ethanol, isopropanol and n-butanol, stirring for 10min, adding acetic acid catalyst and water mixed solution, heating to 40 deg.C, reacting for 30min, adding n-butyl titanate, reacting for 7 hr, cooling to room temperature, adding amino resin, epoxy resin and nano TiO2And (3) continuously stirring the ethanol dispersion liquid (with the solid content of 25 percent and the particle size of 30nm) for 4 hours to obtain the composite polysiloxane protective finish paint for PVD, coating the composite polysiloxane protective finish paint on the PVD aluminized surface, and curing at 120 ℃ for 100min to obtain the film layer performance shown in Table 1.
Example 5
A composite polysiloxane protective finish paint for PVD comprises the following formula (weight percentage):
the preparation and application method comprises the following steps:
adding 3- (methacryloyloxy) propyl trimethoxy silane, phenyl trimethoxy silane, dimethyl dimethoxy silane, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, ethanol and isopropanol solvent into a reaction bottle at room temperature, stirring for 10min, adding a mixed solution of an acetic acid catalyst and water, heating to 45 ℃, reacting for 25min, adding aluminum isopropoxide, continuing to react for 8h, cooling to room temperature, adding amino resin, epoxy resin and nano TiO2And (3) continuously stirring the ethanol dispersion liquid (with the solid content of 30 percent and the particle size of 10nm) for 4 hours to obtain the composite polysiloxane protective finish paint for PVD, coating the composite polysiloxane protective finish paint on the PVD aluminized surface, and curing at 110 ℃ for 120min to obtain the film layer performance shown in Table 1.
Comparative embodiment
The following comparative examples were all set up on the basis of example 4 in the above-described case.
Comparative example 1
The formulation of example 4 was changed to "butyl titanate 5.0, ethanol 18.0" for "butyl titanate 0, ethanol 23.0", otherwise the same as in example 4, and the film properties are shown in table 1.
Comparative example 2
The formulation of example 4, wherein "amino resin 4.0 and ethanol 18.0" was replaced with "amino resin 0 and ethanol 22.0", was otherwise the same as in example 4, the film properties are shown in Table 1.
Comparative example 3
The formulation of example 4 was changed to "epoxy resin 6.0 and ethanol 18.0" and "epoxy resin 0 and ethanol 24.0", the same procedure as in example 4 was repeated, and the film properties are shown in Table 1.
Comparative example 4
The formulation of example 4 was changed to "amino resin 0, epoxy resin 0, ethanol 28.0" instead of "amino resin 4.0, epoxy resin 0, ethanol 28.0", which is otherwise the same as in example 4, and the film properties are shown in table 1.
Comparative example 5
"Nano TiO" in formulation of example 428.0 part of dispersion liquid and 18.0 parts of ethanol are replaced by' nano TiO2Dispersion 0, 26.0' ethanol, otherwise the same as in example 4, film properties are given in Table 1.
TABLE 1 composite polysiloxane protective topcoat for PVD
From comparative examples 1 to 4, it can be seen that if components such as butyl titanate, amino resin, epoxy resin and the like are not used in the formula, the alkali resistance, CASS and the like of polysiloxane are reduced, and from comparative example 5, if nano TiO is not used in the formula2The dispersion, the coating resistance to xenon lamp ageing is also reduced. Finally, it is noted that the above-mentioned list is only a few specific embodiments of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. A composite polysiloxane protective finish paint for PVD is characterized in that the finish paint is prepared by a silane coupling agent, an organic metal precursor, a composite polymer resin, an ultraviolet absorbent and the like after hydrolysis and polycondensation reaction under the action of an acid catalyst, and the specific formula is as follows (in percentage by weight):
2. the composite polysiloxane protective finishing paint for PVD according to claim 1, wherein the silane coupling agent is ethyl orthosilicate, methyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane, n-hexyltrimethoxysilane, n-hexyltriethoxysilane, n-octyltrimethoxysilane, n-octyltriethoxysilane, n-decyltrimethoxysilane, n-decyltriethoxysilane, dodecyltrimethoxysilane, dodecyltriethoxysilane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propyltriethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, 3- (methacryloyloxy) propyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 1, 2-bis (trimethoxy silicon) ethane and bis- [3- (triethoxy silicon) propyl ] -tetrasulfide.
3. The composite polysiloxane protective finishing paint for PVD according to claim 2, characterized in that the silane coupling agent is a compound of ethyl orthosilicate, methyltrimethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, n-propyltrimethoxysilane, isobutyltrimethoxysilane, n-hexyltrimethoxysilane, n-octyltrimethoxysilane, n-decyltrimethoxysilane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, phenyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane and 1, 2-bis (trimethoxy silicon) ethane.
4. The composite polysiloxane protective finishing paint for PVD according to claim 3, characterized in that the silane coupling agent is a compound of a plurality of tetraethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, isobutyltrimethoxysilane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane and phenyltrimethoxysilane.
5. The composite polysiloxane protective finishing paint for PVD according to claim 1, wherein the organic metal precursor is one of ethyl titanate, isopropyl titanate, n-butyl zirconate and aluminum isopropoxide, preferably one of isopropyl titanate, n-butyl titanate and aluminum isopropoxide.
6. The composite polysiloxane protective finishing paint for PVD according to claim 1, characterized in that the polymer resin is one or more of amino resin, hyperbranched polyester resin, epoxy resin and polycarbonate diol, preferably one or two of amino resin and epoxy resin.
7. The composite polysiloxane protective finishing paint for PVD according to claim 1, wherein the ultraviolet absorber is nano TiO2, nano ZnO, nano CeO2 ethanol dispersion, solid content is 15-40%, and particle size is 10-100 nm.
8. The composite polysiloxane protective finishing paint for PVD according to claim 1, wherein the organic solvent is one or more of methanol, ethanol, isopropanol, n-butanol, 2-butanol, propylene glycol methyl ether, ethylene glycol butyl ether and dipropylene glycol methyl ether, preferably one or more of ethanol, isopropanol and n-butanol, and the acid catalyst is one of hydrochloric acid, nitric acid, acetic acid and p-toluenesulfonic acid, preferably one of hydrochloric acid and acetic acid.
9. A preparation method of composite polysiloxane protective finish paint for PVD is characterized by comprising the following steps: adding a silane coupling agent and an organic solvent into a reaction bottle at room temperature, stirring for 10min, adding a mixed solution of an acid catalyst and water, heating to 30-60 ℃, reacting for 20-60 min, adding an organic metal precursor, continuing to react for 6-12 h, cooling to room temperature, adding a polymer resin and an ultraviolet absorbent, and continuing to stir for 2-5 h to obtain the composite polysiloxane protective finish paint for PVD.
10. The preparation method of the composite polysiloxane protective finishing coat for PVD according to claim 9, characterized in that the curing temperature is 80-150 ℃, the curing time is 30-240 min, preferably 100-130 ℃, the curing time is 45-150 min, and the thickness of the cured dry film is 1-10 μm, preferably 3-8 μm; the substrate PVD metal plating layer is made of aluminum, indium, chromium and the like, preferably aluminum, and the film thickness, the adhesive force (grid marking), the alkali resistance (pH 13.5), the CASS and the xenon lamp aging resistance of the substrate PVD metal plating layer are tested by adopting a GMW 1699 standard.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114958155A (en) * | 2022-05-10 | 2022-08-30 | 浙江华普环保材料有限公司 | Silane-containing chromium-free roll priming paint |
| CN115044236A (en) * | 2022-05-31 | 2022-09-13 | 苏州图纳新材料科技有限公司 | Preparation method of corrosion-resistant coating |
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