A kind of acid-resistant and electroplating-resistant ink and preparation method thereof

Abstract

The present invention relates to an anti-acid corrosion and anti-electroplating ink and a preparation method thereof. The ink comprises the following components calculated by weight: 10-20 parts of resin, 24-48 parts of modified silver powder composite sepiolite powder, 1.5-3 parts of dispersant, 0.5-1 parts of leveling agent, 0.8-1.6 parts of defoamer, 0.2-0.6 parts of wetting agent, 0.1-0.5 parts of anti-settling agent, 3-6 parts of curing agent and 60-100 parts of solvent. The present invention adopts a composite resin of acrylic resin and phenoxy resin as the main resin, and the composite resin has better adhesion and heat resistance stability than pure acrylic resin; modified silver powder composite sepiolite powder is used to replace traditional silver powder, which not only has better dispersibility, but also has better improvement in acid corrosion resistance and electroplating resistance; the curing agent is a blocked isocyanate curing agent, which can enhance the storage stability performance of the ink and keep the uniformity of the ink for a long time when it is not used.

Description

Technical Field

[0001] The invention relates to the field of inks, and in particular to an acid-resistant and electroplating-resistant ink and a preparation method thereof. Background Art

[0002] PCB, or printed circuit board, is an important electronic component, a support for electronic components, and also a carrier for the electrical connection of electronic components. PCB ink refers to the ink used for printed circuit boards. Its important physical properties are the viscosity, thixotropy and fineness of the ink. In the manufacturing process of printed circuit boards, screen printing is one of the indispensable and important processes. Therefore, in order to improve the fidelity of image reproduction, the ink must have good viscosity and appropriate thixotropy.

[0003] However, the inks currently on the market generally have the defect of poor anti-plating performance. For example, the electroplating current cannot be too large, which easily causes plating penetration, making it difficult to improve production efficiency. In addition, the existing mirror silver paste inks generally have the problem of short etching time, especially in high-concentration strong acid solutions. The ink layer has an even shorter tolerance time and cannot meet the needs of deep etching products. Summary of the invention

[0004] In view of the problems existing in the prior art, the object of the present invention is to provide an acid-etching and anti-electroplating ink and a preparation method thereof.

[0005] The purpose of the present invention is achieved by the following technical solutions:

[0006] In a first aspect, the present invention provides an acid-resistant and electroplating-resistant ink, which comprises the following components in parts by weight:

[0007] 10-20 parts of resin, 24-48 parts of modified silver powder composite sepiolite powder, 1.5-3 parts of dispersant, 0.5-1 parts of leveling agent, 0.8-1.6 parts of defoamer, 0.2-0.6 parts of wetting agent, 0.1-0.5 parts of anti-settling agent, 3-6 parts of curing agent and 60-100 parts of solvent.

[0008] Preferably, the resin is a mixture of acrylic resin and phenoxy resin, and the mass ratio of acrylic resin to phenoxy resin is 8-12:1.

[0009] Preferably, the acrylic resin is a mixture of one or more of epoxy acrylate resin, styrene acrylic resin, and ethyl acrylate-methyl methacrylate copolymer.

[0010] Preferably, the phenoxy resin is a mixture of one or more of phenoxy resin PKHH, phenoxy resin PKHB and phenoxy resin PKHA.

[0011] More preferably, the phenoxy resin is phenoxy resin PKHB, with a weight average molecular weight of 32,000; and the acrylic resin is styrene acrylic resin, with a brand name of Indurez SR 10.

[0012] Preferably, the preparation method of the modified silver powder composite sepiolite powder comprises:

[0013] S1. Surface treatment of sepiolite powder:

[0014] Weighing sepiolite powder and deionized water, mixing, heating and stirring under the action of silane coupling agent KH-560, filtering and drying to obtain epoxidized sepiolite powder;

[0015] S2. Surface treatment of silver powder:

[0016] Weigh nano silver powder and deionized water, mix them, heat and stir them under the action of silane coupling agent KH-560, filter and dry them to obtain epoxidized silver powder;

[0017] S3. Modification of sepiolite powder:

[0018] Weigh 4,4'-diaminodiphenyl ether and N-methylpyrrolidone, mix them, add epoxidized sepiolite powder, heat and stir to react, and obtain modified sepiolite powder;

[0019] S4. Preparation of modified silver powder composite sepiolite powder:

[0020] Epoxidized silver powder, modified sepiolite powder and N-methylpyrrolidone were weighed and mixed, and after ultrasonic homogenization, the mixture was heated and stirred to react, so as to obtain modified silver powder composite sepiolite powder.

[0021] Preferably, in the S1 process, the temperature of the heating and stirring treatment is 50-70°C, the stirring speed is 150-250r / min, and the stirring time is 4-8h.

[0022] Preferably, in the S1 process, the mass volume ratio of sepiolite powder, silane coupling agent KH-560 and deionized water is 1 g: (0.2-0.8) g: (10-20) mL.

[0023] Preferably, in the S2 process, the mass volume ratio of silver powder, silane coupling agent KH-560 and deionized water is 1 g: (0.1-0.6) g: (10-20) mL.

[0024] Preferably, in the S2 process, the temperature of the heating and stirring treatment is 50-70°C, the stirring speed is 150-250r / min, and the stirring time is 4-8h.

[0025] Preferably, in the S3 process, the mass volume ratio of the epoxidized sepiolite powder, 4,4'-diaminodiphenyl ether and N-methylpyrrolidone is 1 g: (1.15-1.73) g: (10-20) mL.

[0026] Preferably, in the S3 process, the temperature of the heating and stirring reaction is 60-80°C, the stirring speed is 150-250r / min, and the stirring time is 6-10h.

[0027] Preferably, in the S4 process, the mass volume ratio of the modified sepiolite powder, the epoxidized silver powder and the N-methylpyrrolidone is 1 g: (0.48-0.96) g: (10-20) mL.

[0028] Preferably, in the S4 process, the temperature of the heating and stirring reaction is 60-80°C, the stirring time is 8-16h, and the stirring speed is 150-250r / min.

[0029] Preferably, the dispersant is one or more of BASF PX 4585, BASF CX 4230, BASF BASFPX 4701 and BASF PX 4401.

[0030] Preferably, the leveling agent is one or more combinations of organic silicon leveling agent SF-6031, organic silicon leveling agent BY-9315, silicon-free leveling agent HY-2056, silicon-free leveling agent HY-361N, and silicon-free leveling agent HY-495.

[0031] Preferably, the defoaming agent is one or more combinations of SH-Y231, HY-6811, BYK-A555, and BYK-358N.

[0032] Preferably, the wetting agent is one or more combinations of Dow Corning DC-5211, Dow Corning DC-67, Dow Corning DC-51, and Dow Corning DC-29.

[0033] Preferably, the anti-settling agent is one or more combinations of BYK-410, BYK-420, and BYK-430.

[0034] Preferably, the curing agent is a blocked isocyanate curing agent, including one or more combinations of PT-1091, PT-1080Y, and MR-310.

[0035] Preferably, the solvent is one or more combinations of diethylene glycol butyl ether, propylene glycol phenyl ether, glycerol, ethanol, n-butanol, isopropanol, ethyl acetate, butyl acetate, isopropyl acetate, toluene, and xylene.

[0036] In a second aspect, the present invention provides a method for preparing an acid-resistant and electroplating-resistant ink, comprising the following steps:

[0037] Step 1, mixing the resin and the solvent and dispersing them uniformly to obtain a first dispersion;

[0038] Step 2, adding a leveling agent, a defoaming agent, a wetting agent, an anti-settling agent, and a curing agent into the first dispersion, and dispersing them uniformly to obtain a second dispersion;

[0039] Step 3, adding the modified silver powder composite sepiolite powder and the dispersant into the second dispersion liquid, and dispersing them evenly to obtain the acid-corrosion-resistant and electroplating-resistant ink.

[0040] The beneficial effects of the present invention are:

[0041] 1. The present invention prepares an ink with good acid corrosion resistance and electroplating resistance, adopts a composite resin of acrylic resin and phenoxy resin as the main resin, and the composite resin has better adhesion and heat resistance stability than pure acrylic resin; modified silver powder composite sepiolite powder is used to replace traditional silver powder, which not only has better dispersibility, but also has better acid corrosion resistance and electroplating resistance; the curing agent is a blocked isocyanate curing agent, which can enhance the storage stability of the ink and keep the uniformity of the ink for a long time when it is not in use.

[0042] 2. The modified silver powder composite sepiolite powder prepared in the present invention is prepared with sepiolite powder as the matrix and silver powder as the carrier. Different from the traditional load, the present invention first performs surface epoxidation treatment on the sepiolite powder and the silver powder, and then uses 4,4'-diaminodiphenyl ether as an intermediate linker to fix the silver powder on the surface of the sepiolite powder through the amino-epoxy bonding reaction. Among them, the amount of 4,4'-diaminodiphenyl ether added is excessive, so as to ensure sufficient amino content and allow enough epoxidized silver powder to complete the bonding reaction.

[0043] 3. Compared with the traditional sepiolite-loaded silver powder, the modified silver powder composite sepiolite powder obtained by the method of the present invention can not only ensure the uniformity and stability of the silver powder on the sepiolite, but also because the obtained product powder is rich in a variety of chemical groups, such as benzene rings, ether bonds, amine groups, etc., the product powder can have better compatibility in organic solvents and resins, so as to be more evenly dispersed. In addition, it is found through testing that the present invention replaces the traditional silver powder with the modified silver powder composite sepiolite powder, and the acid corrosion resistance and electroplating resistance of the ink are also better improved. DETAILED DESCRIPTION

[0044] The technical solution of the present invention is described below through specific examples. It should be understood that the one or more method steps mentioned in the present invention do not exclude the existence of other method steps before and after the combination step or the insertion of other method steps between these explicitly mentioned steps; it should also be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. Moreover, unless otherwise specified, the numbering of each method step is only a convenient tool for identifying each method step, and is not intended to limit the order of arrangement of each method step or to limit the scope of the present invention. The change or adjustment of the relative relationship thereof shall also be regarded as the scope of the present invention without substantially changing the technical content.

[0045] In order to better understand the above technical scheme, the exemplary embodiments of the present invention are described in more detail below. Although exemplary embodiments of the present invention are shown, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided in order to enable a more thorough understanding of the present invention and to enable the scope of the present invention to be fully communicated to those skilled in the art.

[0046] The particle size of the sepiolite powder used in the embodiment of the present invention is 15-20 μm, and the manufacturer is Lingshou County Huawei Mineral Products Processing Factory. The particle size of the nano silver powder is 20-30 nm, and the manufacturer is Foshan Jinna Technology Co., Ltd.

[0047] The present invention will be further described below in conjunction with the following examples. Example 1

[0048] An acid-resistant and electroplating-resistant ink, calculated by weight, comprises the following components:

[0049] 15 parts of resin, 36 parts of modified silver powder composite sepiolite powder, 2.3 parts of dispersant, 0.7 parts of leveling agent, 1.1 parts of defoamer, 0.4 parts of wetting agent, 0.3 parts of anti-settling agent, 5 parts of curing agent and 80 parts of solvent.

[0050] The resin is a mixture of acrylic resin and phenoxy resin, and the mass ratio of acrylic resin to phenoxy resin is 10: 1. The phenoxy resin is phenoxy resin PKHB, and the weight average molecular weight is 32000; the acrylic resin is styrene acrylic resin, and the brand is Indurez SR 10.

[0051] Among them, the dispersant is BASF PX 4585, the leveling agent is silicone leveling agent SF-603, the defoaming agent is SH-Y231, the wetting agent is Dow Corning DC-5211, and the anti-settling agent is BYK-410.

[0052] The curing agent is a blocked isocyanate curing agent PT-1091, and the solvent is diethylene glycol butyl ether.

[0053] The preparation method of modified silver powder composite sepiolite powder comprises:

[0054] S1, weighing sepiolite powder and deionized water, mixing, homogenizing under the action of ultrasound, adding silane coupling agent KH-560 dropwise, the mass volume ratio of sepiolite powder, silane coupling agent KH-560 and deionized water is 1g:0.5g:15mL, then placing in a water bath, setting the temperature to 60°C, mechanically stirring for 6h, the stirring speed is 200r / min, after the stirring is completed, vacuum filtering out solid powder, washing three times with water, and vacuum drying to obtain epoxidized sepiolite powder;

[0055] S2, weigh silver powder and deionized water, mix them, homogenize them under the action of ultrasound, add silane coupling agent KH-560 dropwise, the mass volume ratio of silver powder, silane coupling agent KH-560 and deionized water is 1g:0.3g:15mL, then place them in a water bath, set the temperature to 60°C, mechanically stir for 6h, and the stirring speed is 200r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain epoxidized silver powder;

[0056] S3, weigh 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone, mix, stir at room temperature until uniform, add epoxidized sepiolite powder, the mass volume ratio of epoxidized sepiolite powder, 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone is 1g:1.44g:10mL, place in a water bath, set the temperature to 70°C, mechanically stir for 8h, the stirring speed is 200r / min, after stirring, vacuum filter out solid powder, wash three times with water, and vacuum dry to obtain modified sepiolite powder;

[0057] S4. Weigh epoxidized silver powder, modified sepiolite powder and N-methylpyrrolidone and mix them. The mass volume ratio of modified sepiolite powder, epoxidized silver powder and N-methylpyrrolidone is 1g:0.72g:15mL. After homogenization under ultrasonic action, place them in a water bath, set the temperature to 70°C, and stir mechanically for 12h at a stirring speed of 200r / min. After stirring, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain modified silver powder composite sepiolite powder.

[0058] The method for preparing the above-mentioned acid-resistant and electroplating-resistant ink comprises the following steps:

[0059] Step 1, mixing the resin and the solvent, and dispersing them uniformly at a speed of 1000 r / min to obtain a first dispersion;

[0060] Step 2, adding a leveling agent, a defoaming agent, a wetting agent, an anti-settling agent, and a curing agent into the first dispersion, and dispersing the mixture uniformly at a speed of 1000 r / min to obtain a second dispersion;

[0061] Step 3, adding the modified silver powder composite sepiolite powder and the dispersant into the second dispersion liquid, and dispersing them uniformly at a speed of 1000 r / min to obtain an acid-resistant and electroplating-resistant ink. Example 2

[0062] An acid-resistant and electroplating-resistant ink, calculated by weight, comprises the following components:

[0063] 10 parts of resin, 24 parts of modified silver powder composite sepiolite powder, 1.5 parts of dispersant, 0.5 parts of leveling agent, 0.8 parts of defoaming agent, 0.2 parts of wetting agent, 0.1 parts of anti-settling agent, 3 parts of curing agent and 60 parts of solvent.

[0064] The resin is a mixture of acrylic resin and phenoxy resin, and the mass ratio of acrylic resin to phenoxy resin is 8: 1. The phenoxy resin is phenoxy resin PKHB, and the weight average molecular weight is 32000; the acrylic resin is epoxy acrylate resin E-20.

[0065] The dispersant is BASF CX 4230, the leveling agent is silicone leveling agent BY-9315, the defoamer is HY-6811, the wetting agent is Dow Corning DC-67, the anti-settling agent is BYK-420, the curing agent is blocked isocyanate curing agent PT-1080Y, and the solvent is propylene glycol phenyl ether.

[0066] Wherein, the preparation method of the modified silver powder composite sepiolite powder is the same as that in Example 1.

[0067] The preparation method of the acid-etching anti-electroplating ink is the same as that of Example 1. Example 3

[0068] An acid-resistant and electroplating-resistant ink, calculated by weight, comprises the following components:

[0069] 12 parts of resin, 35 parts of modified silver powder composite sepiolite powder, 2.1 parts of dispersant, 0.6 parts of leveling agent, 1.2 parts of defoamer, 0.3 parts of wetting agent, 0.2 parts of anti-settling agent, 4 parts of curing agent and 70 parts of solvent.

[0070] The resin is a mixture of ethyl acrylate-methyl methacrylate copolymer and phenoxy resin, and the mass ratio of ethyl acrylate-methyl methacrylate copolymer to phenoxy resin is 9: 1. The phenoxy resin is phenoxy resin PKHB, and the weight average molecular weight is 32,000.

[0071] The dispersant is BASF PX 4701, the leveling agent is silicone-free leveling agent HY-2056, the defoamer is BYK-A555, the wetting agent is Dow Corning DC-51, the anti-settling agent is BYK-430, the curing agent is blocked isocyanate curing agent MR-310, and the solvent is glycerol.

[0072] Wherein, the preparation method of the modified silver powder composite sepiolite powder is the same as that in Example 1.

[0073] The preparation method of the acid-etching anti-plating ink is the same as that of Example 1. Example 4

[0074] An acid-resistant and electroplating-resistant ink, calculated by weight, comprises the following components:

[0075] 20 parts of resin, 48 parts of modified silver powder composite sepiolite powder, 3 parts of dispersant, 1 part of leveling agent, 1.6 parts of defoamer, 0.6 parts of wetting agent, 0.5 parts of anti-settling agent, 6 parts of curing agent and 100 parts of solvent.

[0076] The resin is a mixture of acrylic resin and phenoxy resin, and the mass ratio of acrylic resin to phenoxy resin is 12: 1. The phenoxy resin is phenoxy resin PKHB, and the weight average molecular weight is 32000; the acrylic resin is styrene acrylic resin, and the brand is Indurez SR 10.

[0077] Among them, the dispersant is BASF PX 4401, the leveling agent is the silicone-free leveling agent HY-361N, the defoaming agent is BYK-358N, the wetting agent is Dow Corning DC-29, the anti-settling agent is BYK-410, the curing agent is the blocked isocyanate curing agent MR-310, and the solvent is isopropyl acetate.

[0078] Wherein, the preparation method of the modified silver powder composite sepiolite powder is the same as that in Example 1.

[0079] The preparation method of the acid-etching anti-plating ink is the same as that of Example 1. Example 5

[0080] An acid-resistant and electroplating-resistant ink is different from Example 1 only in that the preparation method of the modified silver powder composite sepiolite powder is different.

[0081] The preparation method of modified silver powder composite sepiolite powder comprises:

[0082] S1. Weigh sepiolite powder and deionized water, mix them, homogenize them under the action of ultrasound, add silane coupling agent KH-560 dropwise, the mass volume ratio of sepiolite powder, silane coupling agent KH-560 and deionized water is 1g:0.2g:10mL, then place them in a water bath, set the temperature to 50°C, mechanically stir for 4h, and the stirring speed is 150r / min. After the stirring is completed, vacuum filter out the solid powder, wash it three times with water, and vacuum dry it to obtain epoxidized sepiolite powder;

[0083] S2, weigh silver powder and deionized water, mix them, homogenize them under the action of ultrasound, add silane coupling agent KH-560 dropwise, the mass volume ratio of silver powder, silane coupling agent KH-560 and deionized water is 1g:0.1g:10mL, then place them in a water bath, set the temperature to 50°C, mechanically stir for 4h, and the stirring speed is 150r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain epoxidized silver powder;

[0084] S3, weigh 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone, mix them, stir them at room temperature until they are uniform, add epoxidized sepiolite powder, the mass volume ratio of epoxidized sepiolite powder, 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone is 1g:1.15g:10mL, place them in a water bath, set the temperature to 60°C, mechanically stir for 6h, and the stirring speed is 150r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain modified sepiolite powder;

[0085] S4. Weigh epoxidized silver powder, modified sepiolite powder and N-methylpyrrolidone and mix them. The mass volume ratio of modified sepiolite powder, epoxidized silver powder and N-methylpyrrolidone is 1g:0.48g:10mL. After homogenization treatment under ultrasonic action, place them in a water bath, set the temperature to 60°C, and mechanically stir for 8h at a stirring speed of 150r / min. After stirring, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain modified silver powder composite sepiolite powder. Example 6

[0086] An acid-resistant and electroplating-resistant ink is different from Example 1 only in that the preparation method of the modified silver powder composite sepiolite powder is different.

[0087] The preparation method of modified silver powder composite sepiolite powder comprises:

[0088] S1. Weigh sepiolite powder and deionized water, mix them, homogenize them under the action of ultrasound, add silane coupling agent KH-560 dropwise, the mass volume ratio of sepiolite powder, silane coupling agent KH-560 and deionized water is 1g:0.8g:20mL, then place them in a water bath, set the temperature to 70°C, mechanically stir for 8h, and the stirring speed is 250r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain epoxidized sepiolite powder;

[0089] S2, weigh silver powder and deionized water, mix them, homogenize them under the action of ultrasound, add silane coupling agent KH-560 dropwise, the mass volume ratio of silver powder, silane coupling agent KH-560 and deionized water is 1g:0.6g:20mL, then place them in a water bath, set the temperature to 70°C, mechanically stir for 8h, and the stirring speed is 250r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain epoxidized silver powder;

[0090] S3, weigh 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone, mix them, stir them at room temperature until they are uniform, add epoxidized sepiolite powder, the mass volume ratio of epoxidized sepiolite powder, 4,4'-diaminodiphenyl ether and N-methyl pyrrolidone is 1g:1.73g:20mL, put them in a water bath, set the temperature to 80°C, mechanically stir for 10h, and the stirring speed is 250r / min. After the stirring is completed, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain modified sepiolite powder;

[0091] S4. Weigh epoxidized silver powder, modified sepiolite powder and N-methylpyrrolidone and mix them. The mass volume ratio of modified sepiolite powder, epoxidized silver powder and N-methylpyrrolidone is 1g:0.96g:20mL. After homogenization treatment under ultrasonic action, place them in a water bath, set the temperature to 80°C, and mechanically stir for 16h at a stirring speed of 250r / min. After stirring, vacuum filter out the solid powder, wash it with water three times, and vacuum dry it to obtain modified silver powder composite sepiolite powder.

[0092] Comparative Example 1

[0093] An ink, which is different from Example 1 only in that the modified silver powder composite sepiolite powder in the ingredients of Example 1 is replaced by ordinary nano silver powder with a particle size of 20-30 nm.

[0094] Comparative Example 2

[0095] An ink, which is different from Example 1 only in that the modified silver powder composite sepiolite powder in the ingredients of Example 1 is replaced by epoxidized silver powder (prepared in the same way as Example 1).

[0096] Comparative Example 3

[0097] An ink, which differs from Example 1 only in that the modified silver powder composite sepiolite powder in the ingredients of Example 1 is replaced by a mixture of ordinary nano silver powder with a particle size of 20-30 nm and sepiolite powder with a particle size of 15-20 μm, and the mass volume ratio of sepiolite powder to silver powder is 1:0.72.

[0098] The ink prepared in Example 1 and Comparative Examples 1-3 was used for printing, and the printing was processed by screen printing process (the mesh number of the screen was 420 meshes, the tension was 22.5N / m, and the thickness was 60μm). The inks of Example 1 and Comparative Examples 1-3 were used for printing, and the curing was carried out at 150℃×30min, and then the performance was tested and compared. Among them, the mirror effect was observed by naked eyes, and the mirror was bright and there was no white fog, which was excellent, otherwise it was not good; the electroplating resistance and acid corrosion resistance were tested with reference to GB / T29846-2013, the electroplating property was copper plating (current density 12ASF, electroplating time 10min), and the etching was etching with acid copper chloride (200g / L) etching solution for 100s; the storage stability test was tested with reference to GB / T 6753.3-1986, the storage temperature was 50℃, and the storage time was 30d. The test results are shown in Table 1.

[0099] Table 1 Performance test results of different inks

[0100] Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Mirror effect excellent Poor excellent Poor Electroplating resistance (copper plating) No plating, no blistering, no shedding There is seepage and blistering, and a lot of shedding There is permeation plating, no blistering, a small amount of shedding There is seepage and blistering, and a lot of shedding Acid corrosion resistance (acid copper chloride etching) The graphics are complete, without erosion or shedding. Some erosion and shedding There is erosion and wrinkling but no shedding Some erosion, no shedding Storage stability pass Not passed pass Not passed

[0101] It can be seen from Table 1 that the ink prepared in Example 1 has excellent mirror effect, excellent electroplating resistance and acid corrosion resistance, and also has good storage stability, which is far better than the performance of various inks in the comparative examples.

[0102] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms should not be understood as necessarily being directed to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine different embodiments or examples described in this specification.

[0103] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.

Claims

1. An acid-resistant and electroplating-resistant ink, characterized in that: Calculated by weight, it includes the following ingredients: 10-20 parts of resin, 24-48 parts of modified silver powder composite sepiolite powder, 1.5-3 parts of dispersant, 0.5-1 parts of leveling agent, 0.8-1.6 parts of defoamer, 0.2-0.6 parts of wetting agent, 0.1-0.5 parts of anti-settling agent, 3-6 parts of curing agent and 60-100 parts of solvent; The resin is a mixture of acrylic resin and phenoxy resin, and the mass ratio of acrylic resin to phenoxy resin is 8-12:1; The preparation method of the modified silver powder composite sepiolite powder comprises: S1, weighing sepiolite powder and deionized water, mixing, heating and stirring under the action of silane coupling agent KH-560, filtering and drying to obtain epoxidized sepiolite powder; S2, weighing nano silver powder and deionized water, mixing, heating and stirring under the action of silane coupling agent KH-560, filtering and drying to obtain epoxidized silver powder; S3, weighing 4,4'-diaminodiphenyl ether and N-methylpyrrolidone, mixing, adding epoxidized sepiolite powder, heating and stirring to react, to obtain modified sepiolite powder; S4, weighing epoxidized silver powder, modified sepiolite powder and N-methylpyrrolidone, mixing them, ultrasonically homogenizing them, heating them and stirring them to react, so as to obtain modified silver powder composite sepiolite powder.

2. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: The acrylic resin is one or more combinations of epoxy acrylate resin, styrene acrylic resin, and ethyl acrylate-methyl methacrylate copolymer; the phenoxy resin is one or more combinations of phenoxy resin PKHH, phenoxy resin PKHB, and phenoxy resin PKHA.

3. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: In the S1 process, the temperature of the heating and stirring treatment is 50-70°C, the stirring speed is 150-250r / min, and the stirring time is 4-8h; the mass volume ratio of sepiolite powder, silane coupling agent KH-560 and deionized water is 1g: (0.2-0.8)g: (10-20)mL.

4. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: In the S2 process, the mass volume ratio of nano silver powder, silane coupling agent KH-560 and deionized water is 1g: (0.1-0.6) g: (10-20) mL; the temperature of the heating and stirring treatment is 50-70° C., the stirring speed is 150-250 r / min, and the stirring time is 4-8 h.

5. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: In the S3 process, the mass volume ratio of epoxidized sepiolite powder, 4,4'-diaminodiphenyl ether and N-methylpyrrolidone is 1g: (1.15-1.73) g: (10-20) mL; the temperature of the heated stirring reaction is 60-80°C, the stirring speed is 150-250 r / min, and the stirring time is 6-10h.

6. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: In the S4 process, the mass volume ratio of modified sepiolite powder, epoxidized silver powder and N-methylpyrrolidone is 1g: (0.48-0.96) g: (10-20) mL; the temperature of the heated stirring reaction is 60-80°C, the stirring time is 8-16h, and the stirring speed is 150-250r / min.

7. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: The dispersant is one or more combinations of BASF PX 4585, BASF CX 4230, BASF PX 4701, and BASF PX 4401; the leveling agent is one or more combinations of silicone leveling agent SF-6031, silicone leveling agent BY-9315, silicone-free leveling agent HY-2056, silicone-free leveling agent HY-361N, and silicone-free leveling agent HY-495; the defoamer is one or more combinations of SH-Y231, HY-6811, BYK-A555, and BYK-358N; the wetting agent is one or more combinations of Dow Corning DC-5211, Dow Corning DC-67, Dow Corning DC-51, and Dow Corning DC-29.

8. The acid-resistant and electroplating-resistant ink according to claim 1, characterized in that: The anti-settling agent is one or more combinations of BYK-410, BYK-420, and BYK-430; the curing agent is a blocked isocyanate curing agent, including one or more combinations of PT-1091, PT-1080Y, and MR-310; the solvent is one or more combinations of diethylene glycol butyl ether, propylene glycol phenyl ether, glycerol, ethanol, n-butanol, isopropanol, ethyl acetate, butyl acetate, isopropyl acetate, toluene, and xylene.

9. A method for preparing the acid-corrosion-resistant and electroplating-resistant ink according to claim 1, characterized in that: The following steps are involved: Step 1, mixing the resin and the solvent and dispersing them uniformly to obtain a first dispersion; Step 2, adding a leveling agent, a defoaming agent, a wetting agent, an anti-settling agent, and a curing agent into the first dispersion, and dispersing them uniformly to obtain a second dispersion; Step 3, adding the modified silver powder composite sepiolite powder and the dispersant into the second dispersion liquid, and dispersing them evenly to obtain the acid-corrosion-resistant and electroplating-resistant ink.