A single-component self-crosslinking type matt insulating black ink and a preparation method thereof

By using a single-component self-crosslinking matte insulating black ink, which forms a tight network structure using self-crosslinking acrylate resin and matting powder, the problems of insufficient solvent resistance, high temperature resistance and insulation of existing matte insulating black inks are solved, and a high-performance ink layer effect is achieved.

CN117050581BActive Publication Date: 2026-03-27CHANGSHU GUOHE NEW MATERIALS CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-08
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Existing technologies cannot simultaneously meet the requirements of matte finish, solvent resistance, high temperature resistance, and insulation for black inks used in insulating packaging of batteries and electronic products, and also suffer from problems such as short service life and easy sticking to the back.

Method used

It adopts a single-component self-crosslinking matte insulating black ink, using self-crosslinking acrylate resin as a binder, combined with organic and inorganic matting powders, carbon black and cellulose, and forms a tight network structure through low-temperature self-crosslinking curing, avoiding the use of ketone solvents and organometallic drying agents.

Benefits of technology

It achieves resistance to wiping with solvents such as ethanol, ethyl acetate, and methyl ethyl ketone in the ink layer, with good adhesion, high flexibility, high temperature resistance, strong insulation, no time restrictions during construction, avoids back-sticking, and reduces costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a single-component self-crosslinking matte insulating black ink and a preparation method thereof. The black ink comprises the following components in parts by mass: a connecting material: 19-50 parts; a dispersing agent: 0.5-5 parts; carbon black: 5-15 parts; extinction powder: 1-10 parts; cellulose: 1-5 parts; and a solvent: 15-73.5 parts. The connecting material is a solvent type self-crosslinking acrylic resin. The single-component self-crosslinking matte insulating black ink solves the problems of short available time, poor storage stability, easy sticking during printing, high construction requirement and waste of residual ink of a double-component system matte insulating black ink, and solves the problems of insufficient solvent resistance and poor high-temperature resistance of a common single-component insulating black ink, and has a good application prospect.
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Description

TECHNICAL FIELD

[0001] The present application relates to a single-component self-crosslinking ink and a preparation method thereof, in particular to a single-component self-crosslinking matte insulating black ink and a preparation method thereof. BACKGROUND

[0002] The insulating packaging of batteries, electronic products and the like prints ink on the PET, PI, NY, PP and the like film after corona treatment in the way of intaglio printing, mainly in black. In order to highlight the visual effect of the text and patterns on the ink layer, the ink layer is required to have a matte effect. During printing, the text and patterns on the ink layer may not meet the quality requirements, at which time the text and patterns on the ink layer need to be wiped off with solvents such as ethanol, ethyl acetate and butanone for re-printing, and the ink layer itself needs to be resistant to solvent wiping and the ink layer cannot be discolored. The black ink suitable for the insulating packaging of batteries, electronic products and the like needs to meet the performance requirements: good flexibility, high temperature resistance, solvent resistance (ethanol, ethyl acetate, butanone), good adhesion, matte (glossiness 1-5), insulation (resistance value > 10 12 Ω), long use time, low-temperature curing (50-60℃), anti-blocking (not sticky after printing and winding). The invention patent (publication number CN110564207A) uses polycarbonate diol resin and hydroxy acrylic resin as the connecting material to make ink, uses organic metal as the catalyst, and adds isocyanate curing agent for curing reaction to meet the performance requirements of resistance to ketone and ester solvents. The invention uses ketone solvents, which is difficult to meet the current environmental friendly requirements of no benzene and no ketone. And it needs to use organic metal catalyst, which is also limited by environmental protection in use. The addition of isocyanate curing agent in the ink is a two-component system, which must be used up within a short time (usually not more than one day), otherwise the remaining ink will become gelatinous and invalid, causing waste. After adding the curing agent in the ink, the phenomenon of sticky back is easy to occur during printing and winding, which affects the quality of the printed product. The invention patent (publication number CN107868510A) uses copolymer polyester resin as the connecting material and ketone solvent to make single-component black insulating matte ink, without using curing agent, the ink can be stored for a long time, which is convenient to use, and has good adhesion and resistance to ethanol and other performances. However, the ink without curing and crosslinking reaction does not form a network crosslinking structure, and the resistance to ester solvents such as ethyl acetate and ketone solvents such as butanone which have stronger dissolving ability than ethanol is insufficient, and the high temperature resistance is also insufficient. The single-component black insulating matte ink is mainly applied to the insulating packaging of batteries, electronic products and the like, and since batteries and electronic products are prone to heat, they need to have high temperature resistance. Since carbon black has conductivity (low resistivity), the resistivity of inorganic matting powder (silicon dioxide) is also not high, so the single-component black ink (black ink) which meets the requirements of matte and insulation and takes into account the resistance to solvents and high temperature has high technical difficulty. SUMMARY

[0003] The present application aims to provide a single-component self-crosslinking matte insulating black ink resistant to wiping with solvents such as ethanol, ethyl acetate and butanone, having flexibility, high temperature resistance, good adhesion, matte, insulation, unlimited use time, anti-blocking (not sticking to the back after printing and rolling), no use of ketone solvents and organic metal drier, and after low-temperature self-crosslinking curing (50-60 DEG C), the surface tension of the ink layer reaches 38 dynes or above, without affecting re-printing or coating other patterns or characters; and another object of the present application is to provide a preparation method of the single-component self-crosslinking matte insulating black ink.

[0004] Technical scheme: The single-component self-crosslinking matte insulating black ink comprises the following components in parts by mass:

[0005] Connecting material: 19-50 parts;

[0006] Dispersing agent: 0.5-5 parts;

[0007] Carbon black: 5-15 parts;

[0008] Matte powder: 1-10 parts;

[0009] Cellulose: 1-5 parts;

[0010] Solvent: 15-73.5 parts

[0011] The connecting material is a single-component self-crosslinking acrylate resin, the acrylate resin itself has a non-linear structure, and there are many points for crosslinking reaction, and after self-crosslinking curing reaction, a more compact multi-dimensional network structure is formed, and the ink layer has flexibility, solvent resistance and high temperature resistance.

[0012] Preferably, the matte powder comprises organic matte powder and inorganic matte powder, the organic matte powder is 0.5-5 parts, and the inorganic matte powder is 0.5-5 parts.

[0013] The resistivity of the carbon black is generally between 10 -12 Ω.m-10 -4 Ω.m, and it belongs to a conductor material. The inorganic matte powder is fumed silica, and it belongs to a semiconductor material. The organic matte powder is polyurea, and it belongs to an insulating material. The connecting material (self-crosslinking acrylate resin) has no ionic bond and no charge, and it belongs to an insulating material. The inorganic matte powder has good matte effect, but it reduces the insulation of the ink coating. The organic matte powder has general matte effect, but it improves the insulation of the ink layer.

[0014] Preferably, X represents the sum of the content of the inorganic matte powder and the content of the carbon black in the black ink, Y represents the sum of the content of the connecting material and the content of the cellulose in the black ink, and X:Y = 1:1-10, so that the ink can simultaneously meet the requirements of matte (glossiness 1-5) and insulation (resistance value >1012 Ω) requirements.

[0015] Preferably, the cellulose has excellent solvent release, which is beneficial to the drying of the ink layer after printing, and does not need to use a drying agent.

[0016] Preferably, the dispersant is one or more of BYK-162, Lubrizol 20000, Lubrizol 24000, Solsperse 771N, Ucar Chemical 9313, BASF P63, and Evonik 4061; the carbon black is one or more of Mitsubishi MA100, MA11, Cabot 99R, 250R, Orion 30L, SB4A, Zhengzhou Tai Rui TR1400, and TR600R; the organic matting powder is one or more of Yaba M2, M3, M5, M7, Zhejiang Jing Tong Technology JJ-3, JJ-4, JJ-5, JJ-5, and JJ-6; the inorganic matting powder is one or more of De Forestas OK500, OK412, TS100, Grace ED80, Eastech E-220A, and Deqing Hengsheng HS-850J; the cellulose is one or more of Eastman cellulose acetate butyrate: CAB-381-0.5, CAB-381-2, CAB-381-0.1, CAB-381-20, CAB-551-0.2, CAB-551-0.01, CAB-381-2BP, CAP-482-0.5, CAB-553-0.4, and CAB-531-1; and the solvent is a mixed solvent of one or more of ethanol, n-propanol, isopropanol, n-butanol, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, and propylene glycol methyl ether acetate.

[0017] Preferably, the raw materials for preparing the connecting material include: a vinyl-based monomer, an alkyl acrylate, a diacetone acrylamide, an initiator, an organic amine, and a solvent; the organic amine is obtained by Michael addition reaction of a bifunctional acrylate monomer with ammonia.

[0018] Preferably, the method for preparing the connecting material includes the following steps:

[0019] (1) A part of the vinyl-based monomer and the solvent are added to the reaction kettle and mixed uniformly, and heated to a reflux state;

[0020] (2) The remaining solution of the vinyl-based monomer, the alkyl acrylate, the diacetone acrylamide, the initiator, and the solvent is added dropwise to the reaction kettle, and the reaction is continued;

[0021] (3) After the reaction is completed, the solvent is added and stirred uniformly, and cooled;

[0022] (4) Add the mixed solution of organic amine and solvent into the prepared acrylate resin, and the solvent type self-crosslinking acrylate resin is obtained after uniform mixing.

[0023] The preparation method of the single-component self-crosslinking matte insulating ink comprises the following steps:

[0024] (1) Mix and uniformly disperse the solvent, connecting material, dispersant, matting powder and carbon black;

[0025] (2) Grind the above materials to obtain the ground ink;

[0026] (3) Mix the cellulose and solvent, add them into the ground ink, uniformly disperse, and filter the material to obtain the single-component self-crosslinking matte insulating black ink.

[0027] Preferably, the fineness of the ground material in step (2) is controlled to be below 10 microns, and the cellulose accounts for 20-30% in the mixed solution of cellulose and solvent in step (3).

[0028] The single-component self-crosslinking matte insulating black ink can be applied on the PET, PI, NY, PP and other films after being treated by corona discharge in the way of gravure printing. The single-component self-crosslinking matte insulating black ink is diluted at a ratio of 100:30-80 with solvent, and is stirred uniformly, and then is used for printing.

[0029] Advantages: Compared with the prior art, the present application has the following remarkable advantages: (1) The single-component self-crosslinking matte insulating black ink solves the problems of short open time, poor storage stability, easy sticking back during printing, high construction requirement and waste of residual ink of the double-component system matte insulating black ink; (2) The single-component self-crosslinking matte insulating black ink solves the problems of insufficient solvent resistance and poor high temperature resistance of the ordinary single-component insulating black ink; (3) Without using the more expensive insulating carbon black, the single-component self-crosslinking matte insulating black ink can also achieve very high insulation performance (resistance value > 10 12 Ω), and reduces the cost. DETAILED DESCRIPTION

[0030] The technical solutions of the present application are further described below in combination with examples.

[0031] Preparation method of connecting material (solvent type self-crosslinking acrylate resin):

[0032] (1) Preparation of organic amine

[0033] Take 2 moles of ammonia water and ethanol solvent into the reactor, stirring, cooling to 5-10℃. Step by step drop 1.1 moles of bifunctional acrylate monomer (ethylene glycol diacrylate or 1,4 butanediol dimethyl acrylate) ethanol solution, reaction at 5-10℃ for 4-6h, restore to room temperature continue to react 3h, get the target product modified organic amine ethanol solution (organic amine content 40%), ready for use.

[0034] The synthetic route of modified organic amine 1 is as follows:

[0035]

[0036] The synthetic route of modified organic amine 2 is as follows:

[0037]

[0038] (2) Preparation of connecting material (solvent type self crosslinking acrylic resin) A

[0039] Add 50 parts of vinyl acetate and 50 parts of ethanol into the reaction kettle and mix uniformly, heat to reflux state; add 30 parts of vinyl acetate, 30 parts of n-butyl acrylate, 38 parts of hydroxypropyl acrylate, 28 parts of ethyl methacrylate, 20 parts of isobornyl methacrylate, 4 parts of diacetone acrylamide, 1.6 parts of azobisisobutyronitrile and 50 parts of ethanol into the reaction kettle after mixing, drop for 5h; after the end of drop, the reaction temperature is kept at reflux state, continue to react for 4h; after the reaction is completed, add 90 parts of ethanol, stir uniformly, cool to below 50℃; mix 6.0 parts of modified organic amine 1 (40% ethanol solution) and 10 parts of ethanol uniformly, add to the prepared acrylate resin, stir uniformly, then discharge, to get connecting material (solvent type self crosslinking acrylic resin) A, solid content 50%, ready for use.

[0040] (3) Preparation of connecting material (solvent type self crosslinking acrylic resin) B

[0041] Add 55 parts of vinyl acetate and 50 parts of ethyl acetate into the reaction kettle and mix uniformly, heat to reflux state; add 35 parts of vinyl acetate, 45 parts of n-butyl acrylate, 25 parts of hydroxyethyl acrylate, 20 parts of ethyl methacrylate, 16 parts of isobornyl acrylate, 4 parts of diacetone acrylamide, 1.2 parts of azobisisobutyronitrile and 50 parts of ethyl acetate into the reaction kettle after mixing, drop for 4h; after the end of drop, the reaction temperature is kept at reflux state, continue to react for 4h; after the reaction is completed, add 80 parts of ethyl acetate, stir uniformly, cool to below 50℃; mix 7.5 parts of modified organic amine 2 (40% ethanol solution) and 20 parts of isopropyl alcohol uniformly, add to the prepared acrylate resin, stir uniformly, then discharge, to get connecting material (solvent type self crosslinking acrylic resin) B, solid content 50%, ready for use.

[0042] Example 1

[0043] 1. Prepare a mixed solvent of ethanol, ethyl acetate, n-propyl acetate and n-butyl acetate in a ratio of 2:2:1:1 at room temperature below 40°C.

[0044] 2. Dissolve cellulose acetate butyrate (Eastman CAB-381-0.1) and the mixed solvent prepared in step 1 into a solution with a mass concentration of 30% by mixing and stirring at room temperature below 40°C (fineness less than 5 microns).

[0045] 3. Add 35 parts of a connecting agent (solvent-based self-crosslinking acrylic resin) A to a tank at room temperature below 40°C, turn on the high-speed disperser at 400 rpm, and then add 30 parts of the mixed solvent of step 1, 2 parts of a dispersant (BYK-162), 4 parts of organic matting powder (Yaba M3), 4 parts of inorganic matting powder (Degussa TS100), and 8 parts of carbon black (Mitsubishi MA11) in sequence while stirring. After the addition is complete, adjust the speed to 1000 rpm and stir for 30 minutes.

[0046] 4. After step 3 is completed, clean the disperser with 3 parts of the mixed solvent prepared in step 1, and transfer the tank to a horizontal sand mill for grinding.

[0047] 5. Perform sand grinding on the above-mentioned materials using a sand mill at room temperature below 40°C. The grinding temperature is controlled below 40°C, and after the fineness is ground to less than 10 microns, clean the sand mill with 8.4 parts of the mixed solvent prepared in step 1, calculate the loss by weight, supplement the loss with the mixed solvent prepared in step 1, and then transfer the tank to a high-speed disperser.

[0048] 6. Add 5 parts of the cellulose acetate butyrate (Eastman CAB-381-0.1) solution prepared in step 2 to the ground material of step 5 at room temperature below 40°C, adjust the stirring speed to 1000 rpm, and stir for 15 minutes. Then filter and package to obtain a self-crosslinking matte insulating black ink.

[0049] 7. When printing, mix the self-crosslinking matte insulating black ink with the mixed solvent prepared in step 1 in a ratio of 100:30-80, stir uniformly, and then use for printing.

[0050] 8. After printing is completed, the printed matter is cured at a temperature of 50°C for 48 hours.

[0051] Example 2

[0052] 1. Prepare a mixed solvent of ethanol, ethyl acetate, n-propyl acetate and n-butyl acetate in a ratio of 2:2:1:1 at room temperature below 40°C.

[0053] 2. Dissolve cellulose acetate butyrate (Eastman CAB-381-0.5) and the mixed solvent prepared in step 1 into a solution with a mass concentration of 20% under stirring at room temperature below 40°C (fineness less than 5 microns).

[0054] 3. Add 40 parts of a connecting agent (solvent-based self-crosslinking acrylic resin) B to a tank under stirring at room temperature below 40°C, and then add 30 parts of the mixed solvent prepared in step 1, 2 parts of a dispersant (Lubrizol 20000), 4 parts of organic matting powder (Yaba M5), 5 parts of inorganic matting powder (Degussa OK-500) and 10 parts of carbon black (Cabot 99R) in sequence under stirring at a speed of 400 rpm. After the addition, the stirring speed is adjusted to 1000 rpm, and the mixture is stirred for 30 minutes.

[0055] 4. After the completion of step 3, clean the disperser with 3 parts of the mixed solvent prepared in step 1, and then transfer the tank to a horizontal sand mill for grinding.

[0056] 5. Grind the above materials using the sand mill under stirring at room temperature below 40°C. The grinding temperature is controlled below 40°C, and the fineness is ground to less than 10 microns. Then, clean the sand mill with 8.4 parts of the mixed solvent prepared in step 1, and calculate the loss. The loss is made up with the mixed solvent prepared in step 1, and then the tank is transferred to a high-speed disperser.

[0057] 6. Add 5 parts of the cellulose acetate butyrate (Eastman CAB-381-0.5) solution prepared in step 2 to the ground materials in step 5, and stir at a speed of 1000 rpm for 15 minutes. Then, filter and package to obtain a self-crosslinking matte insulating black ink.

[0058] 7. When printing, mix the self-crosslinking matte insulating black ink with the mixed solvent prepared in step 1 in a ratio of 100:30-80, and then print after stirring uniformly.

[0059] 8. After printing, the printed matter is cured at a temperature of 50°C for 48 hours.

[0060] Comparative Example 1 (two-component ink)

[0061] 1. Prepare a mixed solvent of methyl ketone and ethyl acetate in a ratio of 3:1 at room temperature below 40°C.

[0062] 2. Under the condition that the room temperature is below 40°C, mix and stir the polycarbonate diol resin PCDLT4692 of Asahi Chemical Industry Co. and the mixed solvent prepared in Step 1 to dissolve into a solution with a solid content of 40% (fineness less than 5 microns) for standby.

[0063] 3. Under the condition that the room temperature is below 40°C, add 20 parts of the resin solution of Step 2 and 15 parts of the hydroxy acrylic resin OLESTER Q850 of Mitsui Chemical into a cylinder, start the high-speed disperser at 400 rpm, and then add the mixed solvent of Step 1, 25 parts, dispersant (BYK-163), 8 parts, flatting powder (Degussa OK-500), 8 parts, and carbon black (Mitsubishi MA11), 8 parts, in sequence while stirring. After the addition, adjust the speed to 1000 rpm and stir for 30 minutes.

[0064] 4. After the completion of Step 3, clean the disperser with 3 parts of the mixed solvent prepared in Step 1, and then transfer the cylinder to a horizontal sand mill for grinding.

[0065] 5. Under the condition that the room temperature is below 40°C, mix and stir the cellulose acetate butyrate (Eastman CAB-381-0.1) and the mixed solvent prepared in Step 1 to dissolve into a solution with a mass concentration of 30% for standby (fineness less than 5 microns).

[0066] 6. Under the condition that the room temperature is below 40°C, grind the above-mentioned materials by using a sand mill. The grinding temperature is controlled below 40°C, and after the fineness is ground to below 10 microns, clean the sand mill with 6.8 parts of the mixed solvent prepared in Step 1, weigh and calculate the loss, supplement the loss with the mixed solvent prepared in Step 1, and then transfer the cylinder to a high-speed disperser.

[0067] 7. Under the condition that the room temperature is below 40°C, add 0.2 parts of the organic tin catalyst T-12 and 5 parts of the cellulose acetate butyrate (Eastman CAB-381-0.1) solution prepared in Step 5 into the ground materials of Step 6, adjust the stirring speed to 1000 rpm, and stir for 15 minutes. Then filter and package to obtain the main body of the two-component matte insulating black ink.

[0068] 8. When printing, mix the main body of the two-component matte insulating black ink, the mixed solvent prepared in Step 1 and the curing agent HUNT-100 of Wanhua in the ratio of 100:30-80:1, stir uniformly, and then print.

[0069] 9. After printing, the printed matter is cured at a temperature of 50°C for 48 hours.

[0070] Comparative Example 2 (non-self-crosslinking ordinary single-component ink)

[0071] 1. Prepare a mixed solvent of butanone: ethyl acetate = 3:1 at room temperature below 40°C and keep it ready for use.

[0072] 2. Mix and stir the copolymerized polyester resin VYLON 673 of Asahi Organic Fibers and the mixed solvent prepared in step 1 to prepare a solution having a solid content of 40% at room temperature below 40°C (fineness less than 5 microns) and keep it ready for use.

[0073] 3. Add 40 parts of the resin solution of step 2 to a tank, turn on a high-speed disperser at 400 rpm, and then add the mixed solvent of step 1 (33 parts), dispersant (BYK-163) (2 parts), matting powder (Degussa OK-500) (2.5 parts), carbon black (Mitsubishi MA11) (1.5 parts), and insulating carbon black (Sylvarl Pigment Chemicals TH-803) (3.5 parts) in this order while stirring. After the completion of the addition, adjust the rotation speed to 1000 rpm and stir for 30 minutes.

[0074] 4. After the completion of step 3, clean the disperser with 3 parts of the mixed solvent prepared in step 1, and transfer the tank to a horizontal sand mill to prepare for grinding.

[0075] 5. Mix and stir cellulose acetate butyrate (Eastman CAB-381-0.1) and the mixed solvent prepared in step 1 to prepare a solution having a mass concentration of 30% at room temperature below 40°C (fineness less than 5 microns) and keep it ready for use.

[0076] 6. Grind the dispersed material of step 3 using a sand mill at room temperature below 40°C. After the grinding to a fineness of less than 10 microns, clean the sand mill with 9.5 parts of the mixed solvent prepared in step 1, weigh the loss, supplement the loss with the mixed solvent prepared in step 1, and then add 5 parts of the cellulose acetate butyrate (Eastman CAB-381-0.1) solution prepared in step 5 to the ground material and transfer it to a high-speed disperser to disperse it uniformly, thereby obtaining a single-component black matte insulating ink.

[0077] 7. When printing, mix the single-component black matte insulating ink and the mixed solvent prepared in step 1 in a ratio of 100:30-80, stir them uniformly, and then use them for printing.

[0078] Performance test:

[0079] 1. Preparation of ink-coated sample sheets for performance test

[0080] (1) Adjust the black inks of the examples and comparative examples to the same solid content (15-25%) with ethanol or ethyl acetate solvent

[0081] (2) Using the printing proofing machine, print the black ink with adjusted solid content on the PET film to make the black ink coating sample with the same wet film thickness.

[0082] (3) After the black ink coating sample is dried by the hair dryer, it is cured at 50°C for 48h, and then taken out for performance test.

[0083] 2. Performance test items and methods

[0084] (1) Adhesion: according to the provisions of GB / T 13217.7-2009 liquid ink adhesion test method, the ink layer is peeled off by 10% or less, which is qualified, the ink layer is peeled off by 5% or less, which is good, and the ink layer is not peeled off, which is excellent;

[0085] (2) Matt: according to the provisions of GB / T 13217.2-2009 liquid ink gloss test method, the gloss between 1-5 is qualified;

[0086] (3) Solvent resistance: according to the provisions of GB / T 23989-2009 paint solvent resistance test method, the solvent resistance is more than 25 times (one way is once), which is qualified;

[0087] (4) Insulation: detected by HIOKI resistance meter, the insulation resistance value is greater than 10 12 Ω is qualified;

[0088] (5) Anti-blocking: according to the provisions of GB / T 13217.8-2009 liquid ink anti-blocking test method, the ink layer is not blocked together, which is qualified;

[0089] (6) Flexibility test

[0090] After drying or curing, the black ink coating sample is folded with ink to ink, and rolled along the folding place for 10 times (one way is one time) at room temperature with 2kg pressure roller. Open the sample, and observe whether there is crack in the self-crosslinking black ink coating at the folding place.

[0091] Judgment standard: unqualified with crack; qualified without crack.

[0092] (7) Temperature resistance test

[0093] Test principle:

[0094] Using the heat sealing instrument with temperature display and control, the highest temperature that the black ink coating sample can withstand is tested to determine the temperature resistance of the black ink.

[0095] Specific method is as follows:

[0096] After drying or curing, the black ink sample is pasted with A4 paper on the ink surface; the temperature of the heat sealing instrument is set, the pressure is 0.3 MPa, and the time is 1 second; the sample is placed on the heat sealing instrument, the PET surface is upward, the upper end of the contact clamp (high temperature heating), the A4 paper is downward, the lower end of the contact clamp, the test key is pressed to start the test, and the sample is taken out after the clamp is loosened; the A4 paper is removed, and whether the black ink on the PET film is transferred to the A4 paper is observed.

[0097] The highest temperature at which the black ink is not transferred to the A4 paper is used to determine the temperature resistance of the sample.

[0098] Determination criteria: below 140 DEG C is unqualified; 140-149 DEG C is qualified; 150-154 DEG C is good; and 155 DEG C and above is excellent.

[0099] (8) Surface tension of the ink layer

[0100] After drying or curing, the black ink coating sample is tested at room temperature with a daoyin pen or daoyin liquid, and the surface tension of the ink surface is 38 dyne or more.

[0101] (9) Ink usable time

[0102] After the ink, the diluent solvent and the curing agent are prepared in proportion and stirred uniformly, they are filled into a transparent glass bottle, sealed, placed in a 40 DEG C constant temperature box, and the time for forming a gel is observed.

[0103] Table 1: Performance test result summary

[0104]

[0105]

[0106] As shown in the data in Table 1, the adhesion, gloss (matte), solvent resistance, insulation resistance, anti-blocking, flexibility, temperature resistance, ink layer surface tension and other properties of the single-component self-crosslinking matte insulating black ink prepared by the present application meet the requirements.

Claims

1. A single-component self-crosslinking matte insulating black ink, characterized in that, The components include the following parts by weight: Connecting material: 19-50 parts; Dispersant: 0.5~5 parts; Carbon black: 5-15 parts; Matte powder: 1-10 parts; Cellulose: 1-5 parts; Organic solvent: 15~73.5 parts; The binder is a solvent-based self-crosslinking acrylic resin, and the raw materials for preparing the binder include: vinyl monomers, alkyl acrylates, diacetone acrylamide, initiators, organic amines, and solvents; The organic amine is a diamine obtained by Michael addition reaction of a bifunctional acrylate monomer with ammonia.

2. The single-component self-crosslinking matte insulating black ink according to claim 1, characterized in that, The matting agent includes organic matting agent and inorganic matting agent, with 0.5 to 5 parts of organic matting agent and 0.5 to 5 parts of inorganic matting agent.

3. The single-component self-crosslinking matte insulating black ink according to claim 2, characterized in that, Let X represent the sum of the content of inorganic matting agent and carbon black in black ink, and Y represent the sum of the content of binder and cellulose in black ink, with X:Y = 1:1-10.

4. The single-component self-crosslinking matte insulating black ink according to claim 1, characterized in that, The method for preparing the binder material includes the following steps: (1) Add some vinyl monomers and solvents to the reaction vessel, mix them evenly, and heat to reflux; (2) The remaining vinyl monomers, alkyl acrylates, diacetone acrylamide, initiator and solvent mixture is added dropwise to the reaction vessel to continue the reaction; (3) After the reaction is complete, add solvent, stir well, and cool; (4) Add the mixed solution of organic amine and solvent to the prepared acrylate resin and mix evenly to obtain the solvent-based self-crosslinking acrylate resin.

5. The single-component self-crosslinking matte insulating black ink according to claim 1, characterized in that, The organic solvent is one or more of ethanol, n-propanol, isopropanol, n-butanol, ethyl acetate, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, and propylene glycol methyl ether acetate.

6. A method for preparing a single-component self-crosslinking matte insulating ink according to any one of claims 1-5, characterized in that, Includes the following steps: (1) Mix and disperse the solvent, binder, dispersant, matting agent and carbon black evenly; (2) Grind the above materials to obtain ground ink; (3) Mix cellulose and solvent, add to the ground ink, disperse evenly, filter and discharge to obtain single-component self-crosslinking matte insulating black ink.

7. The method for preparing the single-component self-crosslinking matte insulating ink according to claim 6, characterized in that, The fineness of the material after grinding in step (2) is controlled to be below 10 micrometers.

8. The method for preparing the single-component self-crosslinking matte insulating ink according to claim 7, characterized in that, In step (3), the cellulose content in the mixture of cellulose and solvent is 20-30%.

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