Glass cover plate pattern ink and preparation method thereof
By using a self-made heat-resistant binder and a modified crosslinking agent to create a crosslinking network, the problem of color change and color spots in glass cover inks at high temperatures was solved, achieving high-precision and high-weather-resistant multi-color printing effects.
Patent Information
- Application Number
- CN202311511009.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-14
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2043-11-14
AI Technical Summary
Existing printing inks for glass covers are prone to discoloration and color spots under high temperature environments, affecting product quality and user experience. Furthermore, multi-color printing requires multiple color passes, and existing technologies cannot meet the requirements for high precision and high weather resistance.
Using a self-made heat-resistant binder and modified crosslinking agent, a highly crosslinked network is formed by crosslinking with the hydroxyl groups on the glass surface. Combined with the chelating properties of the modified crosslinking agent, the adhesion, stability, and high-temperature resistance of the ink are improved.
It achieves stable color retention of ink at high temperatures, maintains good adhesion and color rendering, adapts to multi-color printing needs, and meets the requirements of high-precision and high-weather-resistant glass cover printing.
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Figure BDA0004547351120000101
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of inks, and particularly relates to a glass cover plate pattern ink and a preparation method thereof. BACKGROUND
[0002] With the development of social economy, touch screens are increasingly entering our lives, such as mobile phones, tablets, cars, ATMs, etc. As an important electronic device, general enterprises focus their research on ITO glass, and there is little research on the frame pattern printing process of glass cover plates. The frame pattern of the glass cover plate is generally used for enterprise LOGO and some light transmission indicator light patterns. With the improvement of living standards, people have higher and higher requirements for product quality, and therefore, there is an increasing demand for high-precision and high-weather-resistance glass cover plates, which puts higher requirements on the current printing process. Common glass pattern printing processes include screen printing and UV printing. Screen printing refers to using a silk screen as a plate base and making a silk screen printing plate with graphics by a photosensitive method, and then printing the pattern on the glass. UV printing is a printing process that dries and cures ink through ultraviolet light, which requires ink containing a photosensitizer to cooperate with a UV curing lamp.
[0003] Screen printing technology is simple to master, has low cost and small printing pressure, and is suitable for printing on fragile objects such as glass, has thick ink layers, strong coverage, is not limited by the shape of the printing surface and the size of the area. However, screen printing can only print one color at a time, and multiple passes are required for multi-color printing. UV printing technology can effectively solve this defect. However, existing printing inks are not resistant to high temperatures. For example, in the application of car panels, the temperature inside the car in summer can reach 90℃, and the ink often changes color, seriously affecting product quality and user experience. Long-term research shows that the main reason for the color change of the ink is that the color rendering material in the ink is prone to migration in the ink layer at high temperatures, resulting in local color spots, and is prone to react with the external environment at high temperatures, causing the color rendering material to deteriorate and change color. SUMMARY
[0004] In order to solve the technical problems mentioned in the background art, the purpose of the present application is to provide a glass cover plate pattern ink and a preparation method thereof.
[0005] The purpose of the present application can be achieved by the following technical solutions:
[0006] A glass cover plate pattern ink, comprising by weight parts: temperature-resistant connecting material 35-45 parts, modified crosslinking agent 5.2-6.8 parts, photoinitiator 0.15-0.2 parts, latent curing agent 0.5-0.6 parts, pigment 14-18 parts, titanium white 1.2-1.5 parts, ink oil 18-24 parts, leveling agent 0.6-0.9 parts and defoaming agent 0.2-0.3 parts;
[0007] The temperature-resistant connecting material is prepared by the following method:
[0008] Step A1: mix the amino-terminated silicone oil, triethylamine and tetrahydrofuran, control the temperature in an ice water bath to be 5-15℃, apply low-speed mechanical stirring at 45-60rpm, add methyl vinyl dichlorosilane intermittently, control the total reaction time to be 5-7h, filter and rotary evaporate under reduced pressure after the reaction is completed, quickly remove tetrahydrofuran to avoid the formation of oligomers with high molecular weight, and obtain an oligomeric silicone matrix;
[0009] Further, the ratio of the amino content of the amino-terminated silicone oil, methyl vinyl dichlorosilane, triethylamine and tetrahydrofuran is 0.1mol:0.036-0.042mol:6-9mL:180-250mL, the amino group of the amino-terminated silicone oil reacts with the active chlorine group in the methyl vinyl dichlorosilane to generate an oligomer with a main chain containing a silicon chain;
[0010] Further, the amino-terminated silicone oil is selected from small molecule silicone oil with a room temperature viscosity of not higher than 20mm 2 / s, which is conducive to the mixing of other raw materials and ensures that the viscosity of the finished ink is within a suitable range and adapts to the printing equipment.
[0011] Step A2: mix the oligomeric silicone matrix, epichlorohydrin and dioxane, heat to 55-65℃, apply mechanical stirring at 120-180rpm, and react at constant temperature for 1.5-2.2h, then add sodium hydroxide solution, continue to heat to 80-90℃ and react for 30-50min, cool to room temperature after the reaction is completed, mix with water, remove the aqueous phase, and vacuum dry to obtain the temperature-resistant connecting material;
[0012] Further, the ratio of the oligomeric silicone matrix, epichlorohydrin, sodium hydroxide and dioxane is 50g:0.28-0.36mol:7-10g:80-120mL, the epichlorohydrin preferentially opens the ring with the amine structure in the molecular chain of the oligomeric silicone matrix, and then forms an epoxy structure under the promotion of strong base sodium hydroxide and high temperature conditions.
[0013] The preparation method of the modified crosslinking agent is as follows: isocyanatoethyl methacrylate, pyridine and anhydrous acetone are uniformly mixed under the protection of dry nitrogen, the temperature is controlled at 32-38 DEG C through water bath, mechanical stirring is applied at 180-240 rpm, mercaptoethanol is slowly added, the total addition reaction time is controlled at 2-3 h, acetone is quickly removed through rotary evaporation under reduced pressure after the reaction is completed, the rotary evaporation residue is mixed and washed with water, the aqueous phase is removed, and vacuum drying is carried out to obtain the modified crosslinking agent.
[0014] Further, the usage ratio of isocyanatoethyl methacrylate, mercaptoethanol, pyridine and anhydrous acetone is 0.1 mol:0.1 mol:3-4 mL:40-55 mL, pyridine is used as a weak base catalyst, the alcohol hydroxyl of isocyanatoethyl methacrylate reacts with mercaptoethanol to prepare a methacrylate with a mercapto group.
[0015] Further, the latent curing agent is selected from a polyether amine type curing agent.
[0016] Further, the photoinitiator is selected from photoinitiator 1173.
[0017] A preparation method of a glass cover plate pattern ink comprises the following steps:
[0018] Step S1: temperature-resistant connecting material, pigment, titanium white and leveling agent are added to a grinding machine, and are ground and dispersed at 1200-1500 rpm for 1-1.5 h to obtain a color main agent;
[0019] Step S2: the modified crosslinking agent, the photoinitiator, the latent curing agent, the ink adjusting oil and the defoaming agent are added to a dispersing machine, and are pre-dispersed at 600-800 rpm for 20-30 min, then the color main agent is added and dispersed for 1 h, vacuum defoaming is carried out after filtration to obtain the glass cover plate pattern ink.
[0020] The present application has the following beneficial effects:
[0021] The present application discloses an ink suitable for glass cover plate, which is prepared by using self-made temperature-resistant connecting agent and modified crosslinking agent, and has excellent adhesion and stability. The temperature-resistant connecting agent is prepared by using small molecular amino-terminated silicone oil as base material, introducing unsaturated bond into the silicone chain through substitution reaction with a small amount of methyl vinyl dichlorosilane to form an oligomeric silicone matrix, and then introducing epoxy structure into the side chain by ring opening of epoxy chloropropane and amine structure on the chain, and then closing the ring under the promotion of strong alkali sodium hydroxide and high temperature conditions. The modified crosslinking agent is prepared by reacting isocyanatoethyl methacrylate and mercaptoethanol to form a mercapoto-structured methacrylate. During the curing process of the ink, the epoxy structure of the side chain of the temperature-resistant connecting agent can be crosslinked with the hydroxyl group on the surface of the glass to form primary crosslinking and curing. The connecting agent acts as the matrix of the ink layer and is connected to the glass substrate through covalent bond, so that the ink layer has high adhesion. The molecular main chain is silicone structure, which has good temperature resistance. Importantly, during the curing process, the methacrylate structure in the modified crosslinking agent is crosslinked under the action of ultraviolet initiation, and at the same time, the thiol group in the structure is clicked with the unsaturated structure of the main chain to form secondary crosslinking. On the one hand, a high crosslinking network is formed in the ink layer, which is conducive to improving the overall tolerance of the ink layer. On the other hand, the nitrogen-oxygen-sulfur structure in the crosslinking segment of the modified crosslinking agent has a certain chelating property to the pigment particles, which plays an enveloping effect on the pigment particles during the crosslinking process, reduces the migration of the pigment particles at high temperature and the effect of the external environment, and maintains stable color rendering effect. DETAILED DESCRIPTION
[0022] The technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.
[0023] Embodiment 1
[0024] In this embodiment, the glass cover plate pattern ink is prepared, and the specific implementation process is as follows:
[0025] 1) Preparation of temperature-resistant connecting agent
[0026] Step A1: Take amino-terminated silicone oil, and in this embodiment, KF-8010 type small molecule silicone oil is used, and the room temperature viscosity is about 12mm 2The oligosilicon base was prepared by adding triethylamine and tetrahydrofuran to methylvinyl dichlorosilane provided by Suzhou Jianda Electronics Co., Ltd., controlling the temperature to be 5°C in an ice water bath, applying low-speed mechanical stirring at 45 rpm, taking methylvinyl dichlorosilane and the like in three equal parts, and adding them intermittently for 2 h. After complete addition, constant temperature stirring was continued, the total reaction time of methylvinyl dichlorosilane was controlled to be 7 h, and the ratio of the amino content of the terminal amino silicone oil, methylvinyl dichlorosilane, triethylamine and tetrahydrofuran was 0.1 mol:0.036 mol:6 mL:180 mL. After the reaction was completed, the filtrate was filtered and reduced to 100 Pa or less under reduced pressure, and tetrahydrofuran was quickly removed under high vacuum to obtain the oligosilicon base.
[0027] Step A2: The oligosilicon base, epichlorohydrin and dioxane were mixed, the temperature was raised to 55°C, mechanical stirring was applied at 120 rpm, and constant temperature reaction was carried out for 2.2 h. Sodium hydroxide solution was then added for mixing, the temperature was raised to 80°C, and reaction was continued for 50 min. In the reaction, the ratio of the oligosilicon base, epichlorohydrin, sodium hydroxide and dioxane was 50 g:0.28 mol:7 g:80 mL. After the reaction was completed, the temperature was cooled to room temperature, 2 times the mass of deionized water was added to the reaction substrate for mixing and washing, the aqueous phase was removed, and vacuum drying was carried out to obtain the temperature-resistant connecting material.
[0028] 2) Preparation of modified crosslinking agent
[0029] Methyl methacrylate isocyanide ethyl ester, pyridine and anhydrous acetone were mixed under dry nitrogen protection, the temperature was controlled to be 32°C in a water bath, mechanical stirring was applied at 180 rpm, and then mercaptoethanol was slowly added within 1.5 h. After complete addition, constant temperature stirring was continued, the total addition reaction time of mercaptoethanol was controlled to be 3 h, and the ratio of methyl methacrylate isocyanide ethyl ester, mercaptoethanol, pyridine and anhydrous acetone was 0.1 mol:0.1 mol:3 mL:40 mL. After the reaction was completed, acetone was quickly removed by rotary evaporation under reduced pressure, the rotary evaporation substrate was mixed and washed with water, the aqueous phase was removed, and vacuum drying was carried out to obtain the modified crosslinking agent.
[0030] 3) Preparation of glass cover plate pattern ink
[0031] According to the weight, the raw materials were: 45 parts of the temperature-resistant connecting material prepared in this embodiment and 5.2 parts of the modified crosslinking agent;
[0032] 0.15 parts of a photoinitiator, which was commercially available photoinitiator 1173 in this embodiment, and an industrial grade raw material;
[0033] 0.5 parts of a latent curing agent, which was a polyether amine type curing agent with a model number of Hensmai D400 provided by Guangzhou Yihuisheng Chemical Co., Ltd. in this embodiment;
[0034] 14 parts of a pigment, which was a 78-YT type silver pigment provided by Jizhou County Kewhua Coatings Co., Ltd. in this embodiment;
[0035] Titanium dioxide 1.2 parts, ink grade titanium dioxide was used in the examples, provided by Shandong Zhengyu Chemical Technology Co., Ltd.;
[0036] Printing ink oil 24 parts, ST-1001A type printing ink oil was used in the examples, provided by Guangzhou Yilite Technology Co., Ltd.;
[0037] Leveling agent 0.6 parts, HR-69057 leveling agent was used in the examples, provided by Dongguan Hongrui Chemical Co., Ltd.;
[0038] Defoaming agent 0.2 parts, HR-3117 type defoaming agent was used in the examples, provided by Dongguan Hongrui Chemical Co., Ltd.
[0039] Step S1: The temperature-resistant connecting material, pigment, titanium dioxide and leveling agent were added to the grinder, and were ground and dispersed at 1200 rpm for 1.5 h to obtain a color main agent;
[0040] Step S2: The modified crosslinking agent, photoinitiator, latent curing agent, printing ink oil and defoaming agent were added to the disperser, and were pre-dispersed at 600 rpm for 30 min, then the color main agent was added and dispersed for 1 h, and then filtered and vacuum degassed to obtain a glass cover plate pattern ink.
[0041] Example 2
[0042] The glass cover plate pattern ink was prepared in this example, and the specific implementation process was as follows:
[0043] 1) Preparation of temperature-resistant connecting material
[0044] Step A1: Take amino-terminated silicone oil, AFS-8110 type small molecule silicone oil was used in this example, with a room temperature viscosity of about 15 mm 2 / s, provided by Suzhou Qitian New Material Co., Ltd., add triethylamine and tetrahydrofuran and mix well, control the temperature to be 15℃ in an ice water bath, apply low speed mechanical stirring at 60 rpm, take methyl vinyl dichlorosilane and divide it into three equal parts, add it intermittently for 1.5 h, continue constant temperature stirring after complete addition, control the total reaction time of methyl vinyl dichlorosilane addition to be 5 h, during the reaction, the ratio of amino content of amino-terminated silicone oil, methyl vinyl dichlorosilane, triethylamine and tetrahydrofuran is 0.1 mol:0.042 mol:9 mL:250 mL, after the reaction is completed, filter and reduce the pressure of the filtrate to below 100 Pa, quickly remove the tetrahydrofuran under high vacuum, and obtain an oligomeric silicon matrix.
[0045] Step A2: Take the oligomeric silicon matrix, epichlorohydrin and dioxane, mix well, heat to 65℃, apply 180 rpm mechanical stirring, constant temperature reaction for 1.5 h, then add sodium hydroxide solution and mix, continue to heat to 90℃ for 30 min, in the reaction, the amount ratio of oligomeric silicon matrix, epichlorohydrin, sodium hydroxide and dioxane is 50 g:0.36 mol:10 g:120 mL, after the reaction, cool to room temperature, add 2 times the mass of deionized water to the reaction substrate and mix, remove the aqueous phase, and vacuum dry to obtain the temperature-resistant connecting material.
[0046] 2) Preparation of modified crosslinking agent
[0047] Take isocyanatoethyl methacrylate, pyridine and anhydrous acetone, mix well under dry nitrogen protection, control the temperature of the water bath at 38℃, apply 240 rpm mechanical stirring, then slowly add mercaptoethanol within 1 h, continue to stir at constant temperature after complete addition, control the total addition reaction time of mercaptoethanol to be 2 h, in the reaction, the amount ratio of isocyanatoethyl methacrylate, mercaptoethanol, pyridine and anhydrous acetone is 0.1 mol:0.1 mol:4 mL:55 mL, after the reaction, remove acetone quickly by rotary evaporation under reduced pressure, mix the rotary evaporation substrate with water, remove the aqueous phase, and vacuum dry to obtain the modified crosslinking agent.
[0048] 3) Preparation of glass cover plate pattern ink
[0049] According to the weight, take the raw materials: temperature-resistant connecting material prepared in this embodiment 45 parts and modified crosslinking agent 6.8 parts; photoinitiator 0.2 parts, latent curing agent 0.6 parts, pigment 18 parts, titanium white 1.5 parts, ink oil 18 parts, leveling agent 0.9 parts and defoaming agent 0.3 parts.
[0050] Step S1: Add the temperature-resistant connecting material, pigment, titanium white and leveling agent to the grinder, grind and disperse at 1500 rpm for 1 h to obtain the coloring main agent;
[0051] Step S2: Add the modified crosslinking agent, photoinitiator, latent curing agent, ink oil and defoaming agent to the disperser, pre-disperse at 800 rpm for 20 min, then add the coloring main agent and disperse for 1 h, vacuum degassing after filtration to obtain the glass cover plate pattern ink.
[0052] Example 3
[0053] In this embodiment, the glass cover plate pattern ink is prepared, and the specific implementation process is as follows:
[0054] 1) Preparation of temperature-resistant connecting material
[0055] Step A1: Take the end amino silicone oil (AFS-8110) and add triethylamine and tetrahydrofuran, mix well, control the temperature at 10°C in an ice water bath, apply low-speed mechanical stirring at 55 rpm, take methyl vinyl dichlorosilane and divide it into three equal parts, add it intermittently for 1.8 h, continue constant temperature stirring after complete addition, control the total reaction time of methyl vinyl dichlorosilane addition to be 6 h, in the reaction, the ratio of the amino content of the end amino silicone oil, methyl vinyl dichlorosilane, triethylamine and tetrahydrofuran is 0.1 mol:0.04 mol:8 mL:220 mL, after the reaction is completed, filter and reduce the pressure to below 100 Pa, quickly remove the tetrahydrofuran under high vacuum, and prepare the oligosilicon matrix.
[0056] Step A2: Take the oligosilicon matrix, epichlorohydrin and dioxane, mix and add, heat to 60°C, apply mechanical stirring at 180 rpm, constant temperature reaction for 1.8 h, then add sodium hydroxide solution and mix, continue to heat to 85°C for 40 min, in the reaction, the ratio of the oligosilicon matrix, epichlorohydrin, sodium hydroxide and dioxane is 50 g:0.32 mol:8 g:110 mL, after the reaction is completed, cool to room temperature, add 2 times the mass of deionized water to the reaction substrate and mix, remove the aqueous phase, and vacuum dry to prepare the temperature-resistant connecting material.
[0057] 2) Preparation of modified crosslinking agent
[0058] Take isocyanatoethyl methacrylate, pyridine and anhydrous acetone, mix well under dry nitrogen protection, control the temperature at 35°C in a water bath, apply mechanical stirring at 240 rpm, then slowly add mercaptoethanol in 1.2 h, continue constant temperature stirring after complete addition, control the total addition reaction time of mercaptoethanol to be 2.5 h, in the reaction, the ratio of isocyanatoethyl methacrylate, mercaptoethanol, pyridine and anhydrous acetone is 0.1 mol:0.1 mol:4 mL:50 mL, after the reaction is completed, quickly remove the acetone by rotary evaporation under reduced pressure, mix the rotary evaporation substrate with water, remove the aqueous phase, and vacuum dry to obtain the modified crosslinking agent.
[0059] 3) Preparation of glass cover plate pattern ink
[0060] According to the weight, take the raw materials: temperature-resistant connecting material prepared in this embodiment 42 parts and modified crosslinking agent 6.2 parts; photoinitiator 0.18 parts, latent curing agent 0.5 parts, pigment 15 parts, titanium white 1.4 parts, ink adjusting oil 20 parts, leveling agent 0.7 parts and defoaming agent 0.3 parts.
[0061] Step S1: Add the temperature-resistant connecting material, pigment, titanium white and leveling agent to the grinder, grind and disperse at 1200 rpm for 1.5 h to obtain the coloring main agent;
[0062] Step S2: The modified crosslinking agent, photoinitiator, latent curing agent, ink thinner and defoaming agent were added into a disperser, pre-dispersed for 20 min at 800 rpm, then the colorant main agent was added and dispersed for 1 h, filtered, vacuum degassed to obtain the glass cover plate pattern ink.
[0063] Comparative Example 1
[0064] The commercially available glass special epoxy ink was selected for the present comparative example, and the specific product was 7226 silver Marken ink provided by Dongguan Zaideng Printing Equipment Co., Ltd.
[0065] Comparative Example 2
[0066] The commercially available glass silk screen printing ink was selected for the present comparative example, and the specific product was JMY-9100 mirror surface silver ink provided by Shenzhen Sunflower Electronic Material Co., Ltd.
[0067] In order to verify the related performance of the above inks, each ink was printed on the surface of ITO glass, and the specific operation was as follows:
[0068] The ITO glass was immersed in 5% sodium carbonate solution for 10 min to remove oil and ester, then ultrasonically immersed in ethanol for 5 min, and dried to obtain clean slides;
[0069] The inks of Examples 1-3 and Comparative Example 1 were directly printed on the surface of clean slides, and in the process of Comparative Example 2, 3M primer AP115 primer was first sprayed on the surface of clean slides, and pre-baked at 40℃ for 30 min, then printed by screen printing, and the ink layer thickness was controlled to be 3 μm during the process, then placed in the ultraviolet curing box, and the ultraviolet irradiation intensity was controlled to be 200 W / m 2 , the baking temperature was set as: 80℃, 30 min, 120℃, 10 min, the furnace was cooled to 60℃, and then air-cooled to room temperature to obtain the ink-covered sample.
[0070] The ink-covered sample was used as the sample object, and the related tests on the ink-covered surface state were carried out, which specifically included:
[0071] Water resistance test: according to GB / T 1733-1993 standard, the immersion method was used, and the sample was immersed in water at room temperature for 48 h;
[0072] Acid and alkali resistance test: according to GB / T 9274-1988 standard, sodium hydroxide solution with pH value of 12 and sulfuric acid solution with pH value of 5 were used as test liquids, and the immersion method was used, and the test time was 12 h;
[0073] Adhesion test: according to ASTM D3359-09 standard, the line spacing was 1 mm;
[0074] The related test data is shown in Table 1:
[0075] Table 1
[0076] Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Water resistance No change No change No change No change No change Acid resistance No change No change No change No change Small amount of peeling Alkali resistance No change No change No change No change Small amount of peeling Adhesion 5B 5B 5B 4B 4B
[0077] From the data in Table 1, it can be seen that the ink prepared by the present application has good water resistance, acid resistance and alkali resistance after curing, which meets the printing needs of most glass cover plates, and the adhesion reaches 5B level, which is significantly better than the existing ink.
[0078] To verify the temperature resistance of the ink, according to the GB / T 250-2008 standard, the color difference of the ink after temperature resistance treatment was detected, which was used to characterize the temperature resistance stability of the ink. The temperature resistance stability of the ink was simulated at 85 DEG C for a conventional heat environment and at 170 DEG C for an overheating condition, and the test time was 48h and 30min, respectively. The specific test data are shown in Table 2.
[0079] Table 2
[0080]
[0081] From the data in Table 2, it can be seen that the ink prepared by the present application has good water resistance, acid resistance and alkali resistance after curing, which meets the printing needs of most glass cover plates, and the adhesion reaches 5B level, which is significantly better than the existing ink.
[0082] In the description of the specification, the description of the reference terms "one embodiment", "example", "specific example" and the like means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are contained in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0083] The above is only an example and description of the present application, and those skilled in the art can make various modifications or supplements or use similar ways to replace the described specific embodiments, as long as they do not deviate from the invention or exceed the scope defined by the present claims, which shall belong to the protection scope of the present application.
Claims
1. A glass cover plate pattern ink, characterized by, By weight parts, including: temperature resistant connecting material 35-45 parts, modified crosslinking agent 5.2-6.8 parts, photoinitiator 0.15-0.2 parts, latent curing agent 0.5-0.6 parts, pigment 14-18 parts, titanium dioxide 1.2-1.5 parts, ink oil 18-24 parts, leveling agent 0.6-0.9 parts and defoaming agent 0.2-0.3 parts; The temperature resistant connecting material is prepared by the following method: Step A1: the amino-terminated silicone oil, triethylamine and tetrahydrofuran are uniformly mixed, the temperature is controlled at 5-15℃ in an ice water bath, methyl vinyl dichlorosilane is added in stirring and intermittence, the total reaction time is controlled at 5-7h, after the reaction is completed, the tetrahydrofuran is removed by rotary evaporation under reduced pressure, and an oligomeric silicon matrix is obtained; Step A2: the oligomeric silicon matrix, epichlorohydrin and dioxane are uniformly mixed, the temperature is raised to 55-65℃, stirring is carried out at constant temperature for 1.5-2.2h, sodium hydroxide solution is then added for mixing, the temperature is further raised to 80-90℃ for reaction for 30-50min, after the reaction is completed, the temperature is cooled to room temperature, water is mixed and washed, the aqueous phase is removed, and vacuum drying is carried out, to obtain the temperature resistant connecting material; The preparation method of the modified crosslinking agent is as follows: isocyanatoethyl methacrylate, pyridine and anhydrous acetone are uniformly mixed under dry nitrogen protection, the temperature is controlled at 32-38℃ in a water bath, mercaptoethanol is slowly added in stirring, the total reaction time is controlled at 2-3h, after the reaction is completed, the acetone is removed by rotary evaporation under reduced pressure, the rotary evaporation residue is mixed and washed with water, the aqueous phase is removed, and vacuum drying is carried out, to obtain the modified crosslinking agent.
2. The glass cover plate pattern ink according to claim 1, wherein, The amount ratio of the amino content of the amino-terminated silicone oil, methyl vinyl dichlorosilane, triethylamine and tetrahydrofuran is 0.1mol:0.036-0.042mol:6-9mL:180-250mL.
3. The glass cover plate pattern ink according to claim 2, characterized in that, The end-amino silicone oil is a small molecule silicone oil, and the room temperature viscosity is not higher than 20 mm 2 / s.
4. The glass cover plate pattern ink according to claim 3, characterized in that, The amount ratio of the oligomeric silicon matrix, epichlorohydrin, sodium hydroxide and dioxane is 50g:0.28-0.36mol:7-10g:80-120mL.
5. The glass cover plate pattern ink according to claim 1, wherein The amount ratio of isocyanatoethyl methacrylate, mercaptoethanol, pyridine and anhydrous acetone is 0.1mol:0.1mol:3-4mL:40-55mL.
6. The glass cover plate pattern ink according to claim 1, wherein The latent curing agent is a polyether amine type curing agent.
7. The glass cover plate pattern ink according to claim 1, wherein The photoinitiator is photoinitiator 1173.
8. The method for preparing a patterned ink for a glass cover plate according to claim 1, characterized in that, The method comprises the following steps: Step S1: the temperature resistant connecting material, pigment, titanium dioxide and leveling agent are added to a grinder, and grinding and dispersion are carried out to obtain a coloration main agent; Step S2: the modified crosslinking agent, photoinitiator, latent curing agent, ink oil and defoaming agent are added to a disperser for pre-dispersion, the coloration main agent is then added for mixing and dispersion, vacuum defoaming is carried out after filtration, and a glass cover plate pattern ink is obtained.
Citation Information
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