Preparation method of special high-temperature-resistant and yellowing-resistant solder resist ink for vehicle-mounted PCB (Printed Circuit Board)

Abstract

The invention relates to a preparation method of high-temperature-resistant and yellowing-resistant solder-resistant ink special for a vehicle-mounted PCB (Printed Circuit Board), belonging to the technical field of ink. The preparation method comprises the following steps: uniformly stirring and mixing a binder, varnish, a pigment, modified nano calcium carbonate, a flatting agent and a defoaming agent, grinding and sieving to obtain the high-temperature-resistant and yellowing-resistant solder-resistant ink special for the vehicle-mounted PCB. The bright modified nano calcium carbonate disclosed by the invention is prepared by the following steps: carrying out heating reaction on ethanol, nano calcium carbonate and allyloxytrimethylsilane; the preparation method comprises the following steps: adding 5-norbornene-2-formamide and dioctadecylamine, adjusting the pH value to 10 by using sodium hydroxide, stirring for reaction, filtering, drying, grinding and sieving to obtain the product. The ink prepared by the invention has good fineness, fluidity and glossiness.

Description

Technical Field

[0001] This invention relates to the field of ink technology, and in particular to a method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs. Background Technology

[0002] In the ink production process, pigments are in powder form and binders are in resin-based fluid form. The dispersion of pigments in the binder will affect the ink's fineness, flowability, and gloss.

[0003] Chinese Patent CN113134423A: This invention relates to a method for preparing water-based printing ink, which uses a water-based printing ink preparation device. The device includes a preparation box, a grinding mechanism, a sieving mechanism, a scraping mechanism, and a collection box. The preparation box has a rectangular structure, and the grinding mechanism, sieving mechanism, and collection box are arranged sequentially from top to bottom on the inner wall of the preparation box. The scraping mechanism is provided on the grinding mechanism.

[0004] Chinese Patent CN116036968A discloses a water-based ink preparation process. The specific steps of the preparation process are as follows: water-soluble resin is added to a mixing device and stirred to obtain ink raw materials. Color paste, additives and solvents are added to the mixing device containing the ink raw materials and stirred and mixed evenly. The mixing device includes a mixing drum and a base located at the bottom of the mixing drum.

[0005] Chinese Patent CN113750902A: Belonging to the field of ink preparation, specifically an environmentally friendly water-based printing ink preparation process, including the following steps: S1, Raw material conveying: A conveying mechanism can simultaneously convey multiple different raw materials in equal quantities intermittently, and store them in a mixing tank; S2, Heating and mixing: In step S1, the conveying mechanism drives a high-efficiency mixing mechanism inside the mixing tank, thereby heating and mixing the various raw materials inside the mixing tank; S3, Waste gas treatment: In step S2, the high-efficiency mixing mechanism drives a filtration mechanism inside the mixing tank, thereby automatically purifying the toxic gases generated inside the mixing tank.

[0006] The inks prepared using the above patents and existing technologies have high production costs and their gloss needs further improvement. Summary of the Invention

[0007] To address the above problems, this invention provides a method for preparing a high-temperature resistant and yellowing-resistant solder resist ink specifically for automotive PCBs, the steps of which are as follows: By weight, 55-75 parts of binder, 1-5 parts of ink thinner, 1-5 parts of pigment, 5-15 parts of gloss-modified nano calcium carbonate, 1-5 parts of leveling agent, and 1-5 parts of defoamer are mixed evenly, ground, and sieved to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs.

[0008] Furthermore, the binder is one of acrylate, polyamide resin, and epoxy resin.

[0009] Furthermore, the ink mixing oil is either No. 6 ink mixing oil produced by Henan Innovation Printing Equipment Co., Ltd. or No. 3 ink mixing oil produced by Hangzhou Lengnuan Culture and Art Co., Ltd.

[0010] Furthermore, the pigment is one of titanium dioxide, cobalt green, carbon black, iron oxide, titanium dioxide, cobalt green, carbon black, iron oxide, and phthalocyanine blue.

[0011] Furthermore, the leveling agent is one of silicone oil, polydimethylsiloxane, polymethylalkylsiloxane, or polyether polyester modified organosiloxane.

[0012] Furthermore, the defoamer is one of the following: emulsified silicone oil, higher carbon alcohol fatty acid ester complex, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene alcohol ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether, and polydimethylsiloxane.

[0013] Furthermore, the grinding time is 60-80 minutes.

[0014] Furthermore, the stirring and mixing temperature is 60-80℃, and the time is 50-70 minutes.

[0015] Furthermore, the preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 80-120 parts of nano-calcium carbonate and 3-6 parts of allyloxytrimethylsilane to 1000-1500 parts of ethanol by weight, heat to 60-80℃, sonicate for 30-60 min, and react for 60-90 min. T2: Add 2-5 parts of 5-norbornene-2-carboxamide and 0.5-2 parts of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 60-80℃ for 100-120 min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

[0016] Reaction mechanism: Allyloxytrimethylsilane treatment: Nucleophilic substitution of hydroxyl groups on the surface of nano-calcium carbonate with allyloxytrimethylsilane introduces alkenyl groups onto its surface.

[0017] Amino-olefin addition: Under alkaline conditions, the amino groups of dioctadecylamine and 5-norbornene-2-carboxamide attack the alkenyl double bond, causing norbornene and dioctadecyl to attach to the surface of nano-calcium carbonate.

[0018] Technical effects: This invention discloses a method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs. Compared with existing technologies, this invention has the following significant advantages: 1. Improve dispersion Organic groups, such as norbornene and dioctadecyl groups, are attached to the surface of nano-calcium carbonate. These organic groups increase the compatibility of nano-calcium carbonate with the organic components in the ink, making the ink coating surface smoother, thereby improving the specular reflectivity of light and enhancing the gloss of the ink.

[0019] 2. Enhance surface smoothness Dioctadecyl groups, long-chain alkyl groups, form a relatively soft and smooth outer shell on the surface of nano-calcium carbonate, making the coating surface smoother. A smooth surface reflects light better, producing a high-gloss visual effect.

[0020] 3. Increase the leveling properties of the ink Norbornene groups have a certain rigidity and spatial structure, which can adjust the rheological properties of ink. The ink can spread quickly on the surface of the object and form a uniform coating, avoiding defects such as flow marks and orange peel, thereby improving the smoothness and gloss of the coating. Detailed Implementation

[0021] To further illustrate the technical means and effects adopted by the present invention in order to achieve the intended purpose, the following detailed description is provided in conjunction with embodiments and comparative examples: 1. Fineness test: The fineness shall be determined in accordance with GB / T13217.3-2022.

[0022] 2. Flowability test: The test shall be conducted in accordance with GB / T14624.3-2008.

[0023] 3. Gloss test: The gloss is measured using a gloss meter.

[0024] Example 1 A method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs, comprising the following steps: Mix 55g of binder, 1g of ink thinner, 1g of pigment, 5g of gloss-modified nano-calcium carbonate, 1g of leveling agent, and 1g of defoamer until homogeneous. Then grind and sieve to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs.

[0025] The binder is BR-73 acrylate.

[0026] The ink blending oil mentioned is No. 6 ink blending oil produced by Henan Innovation Printing Equipment Co., Ltd.

[0027] The pigment in question is titanium dioxide.

[0028] The leveling agent is silicone oil.

[0029] The defoamer mentioned is emulsified silicone oil.

[0030] The grinding time is 60 minutes.

[0031] The mixing temperature is 60℃ and the mixing time is 50 minutes.

[0032] The preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 80g of nano-calcium carbonate and 3g of allyloxytrimethylsilane to 1000g of ethanol, heat to 60℃, sonicate for 30min, and then react for 60min. T2: Add 2g of 5-norbornene-2-carboxamide and 0.5g of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 60℃ for 100min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

[0033] Example 2 A method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs, comprising the following steps: Mix 60g of binder, 2g of ink oil, 2g of pigment, 8g of gloss-modified nano calcium carbonate, 2g of leveling agent, and 2g of defoamer until homogeneous. Then grind and sieve to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs.

[0034] The binder is polyamide resin PA6.

[0035] The ink blending oil mentioned is No. 6 ink blending oil produced by Henan Innovation Printing Equipment Co., Ltd.

[0036] The pigment in question is cobalt green.

[0037] The leveling agent is polydimethylsiloxane.

[0038] The defoamer is a high-carbon alcohol fatty acid ester complex.

[0039] The grinding time is 65 minutes.

[0040] The mixing temperature is 65℃ and the mixing time is 55 minutes.

[0041] The preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 90g of nano-calcium carbonate and 4g of allyloxytrimethylsilane to 1100g of ethanol, heat to 65℃, sonicate for 40min, and then react for 70min. T2: Add 3g of 5-norbornene-2-carboxamide and 1g of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 65℃ for 105min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

[0042] Example 3 A method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs, comprising the following steps: 70g of binder, 4g of ink thinner, 4g of pigment, 13g of gloss-modified nano calcium carbonate, 4g of leveling agent, and 4g of defoamer are mixed evenly, ground, and sieved to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs.

[0043] The binder is polyamide resin PA66.

[0044] The ink oil mentioned is No. 3 ink oil from Hangzhou Lengnuan Culture and Art Co., Ltd.

[0045] The pigment in question is carbon black.

[0046] The leveling agent is polymethylalkylsiloxane.

[0047] The defoamer is polyoxyethylene polyoxypropylene pentaerythritol ether.

[0048] The grinding time is 75 minutes.

[0049] The mixing temperature is 75℃ and the mixing time is 65 minutes.

[0050] The preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 110g of nano-calcium carbonate and 5g of allyloxytrimethylsilane to 1400g of ethanol, heat to 75℃, sonicate for 50min, and then react for 80min. T2: Add 4g of 5-norbornene-2-carboxamide and 1.5g of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 75℃ for 115min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

[0051] Example 4 A method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs, comprising the following steps: 75g of binder, 5g of ink thinner, 5g of pigment, 15g of gloss-modified nano-calcium carbonate, 5g of leveling agent, and 5g of defoamer are mixed evenly, ground, and sieved to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs.

[0052] The binder is epoxy resin E44.

[0053] The ink oil mentioned is No. 3 ink oil from Hangzhou Lengnuan Culture and Art Co., Ltd.

[0054] The pigment mentioned is phthalocyanine blue.

[0055] The leveling agent is a polyether polyester modified organosiloxane.

[0056] The defoamer is polydimethylsiloxane.

[0057] The grinding time is 80 minutes.

[0058] The mixing temperature is 80℃ and the mixing time is 70 minutes.

[0059] The preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 120g of nano-calcium carbonate and 6g of allyloxytrimethylsilane to 1500g of ethanol, heat to 80℃, sonicate for 60min, and then react for 90min. T2: Add 5g of 5-norbornene-2-carboxamide and 2g of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 80℃ for 120min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

[0060] Comparative Example 1 No modification was performed on the nano-calcium carbonate; otherwise, it was the same as in Example 1.

[0061] Comparative Example 2 Without adding 5-norbornene-2-carboxamide, otherwise the same as in Example 1.

[0062] Comparative Example 3 Without adding dioctadecylamine, otherwise the same as in Example 1.

[0063] The test results of the examples and comparative examples are shown in Table 1.

[0064] Table 1 Based on the data analysis of the above embodiments and comparative examples, the high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs prepared by the present invention has good fineness, flowability and gloss.

[0065] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs, comprising the following steps: By weight, 55-75 parts of binder, 1-5 parts of ink thinner, 1-5 parts of pigment, 5-15 parts of gloss modified nano calcium carbonate, 1-5 parts of leveling agent, and 1-5 parts of defoamer are mixed evenly, ground, and sieved to obtain a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs. The bright modified nano-calcium carbonate is prepared by reacting nano-calcium carbonate, allyloxytrimethylsilane, 5-norbornene-2-carboxamide, and dioctadecylamine.

2. The preparation method of a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The binder is one of acrylate, polyamide resin, or epoxy resin.

3. The preparation method of a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The ink mixing oil mentioned is No. 6 ink mixing oil produced by Henan Innovation Printing Equipment Co., Ltd. or No. 3 ink mixing oil produced by Hangzhou Lengnuan Culture and Art Co., Ltd.

4. The preparation method of a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The pigment is one of titanium dioxide, cobalt green, carbon black, iron oxide, titanium dioxide, cobalt green, carbon black, iron oxide, and phthalocyanine blue.

5. The preparation method of a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The leveling agent is one of silicone oil, polydimethylsiloxane, polymethylalkylsiloxane, or polyether polyester modified organosiloxane.

6. The method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The defoamer is one of the following: emulsified silicone oil, high carbon alcohol fatty acid ester complex, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene alcohol amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether, and polydimethylsiloxane.

7. The method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The grinding time is 60-80 minutes.

8. The method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The mixing temperature is 60-80℃ and the time is 50-70 minutes.

9. The method for preparing a high-temperature resistant and yellowing-resistant solder resist ink for automotive PCBs according to claim 1, characterized in that: The preparation method of the aforementioned bright modified nano-calcium carbonate is as follows: T1: Add 80-120 parts of nano-calcium carbonate and 3-6 parts of allyloxytrimethylsilane to 1000-1500 parts of ethanol by weight, heat to 60-80℃, sonicate for 30-60 min, and react for 60-90 min. T2: Add 2-5 parts of 5-norbornene-2-carboxamide and 0.5-2 parts of dioctadecylamine, adjust the pH to 10 with sodium hydroxide, stir and react at 60-80℃ for 100-120 min, filter, dry, grind, and sieve to obtain bright modified nano calcium carbonate.

Images