Anti-seepage additive for ink-jet printing as well as synthesis method and anti-seepage process of anti-seepage additive

By developing an anti-seepage additive for inkjet printing, the reaction of compounds A and B generates additives with low surface tension and hydrophilic groups, the problem of spontaneous diffusion of printing ink is solved, and the inkjet printing accuracy and environmental protection and efficiency of the process are improved.

CN120209633APending Publication Date: 2025-06-27上海天承化学有限公司
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Patent Information

Application Number
CN202510370978.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-27
Publication Date
2025-06-27

AI Technical Summary

Technical Problem

The existing welding prevention process has environmental problems, long time, many equipment and high energy consumption, and the low surface tension of the printing ink leads to spontaneous diffusion of the ink, affecting the ink printing accuracy.

Method used

An anti-seepage additive for inkjet printing was developed to produce an anti-seepage additive for inkjet printing with low surface tension and hydrophilic groups through the reaction of compound A (amino-containing polysiloxane) and compound B (a compound containing acryloyloxy or epoxy) to form an anti-seepage additive for inkjet printing with low surface tension and hydrophilic groups. It is used to treat the surface of the substrate, reduce its surface energy and inhibit ink diffusion.

Benefits of technology

It effectively inhibits the spontaneous diffusion of printing ink on the surface of the substrate, improves the inkjet printing accuracy, and has good stability and binding force of anti-seepage agent, which is suitable for large-scale manufacturing.

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Abstract

The invention provides an anti-seepage additive for ink-jet printing as well as a synthesis method and an anti-seepage process of the anti-seepage additive. Synthetic raw materials of the anti-seepage additive for ink-jet printing comprise a compound A and a compound B, the compound A is polysiloxane containing amino groups; and the compound B is a compound containing an acryloyloxy group or a compound containing an epoxy group. A layer of molecular film is adsorbed on the surface of a base material treated by an anti-seepage working solution prepared from the anti-seepage additive for ink-jet printing provided by the invention, so that the surface energy of the base material is reduced, the diffusion of jet printing ink on the surface of the base material can be inhibited, and the ink-jet printing precision is improved; the anti-seepage additive for ink-jet printing does not generate negative effects on the binding force of jet printing ink and the surface of a base material, and has high reliability and high stability.
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Description

Technical Field

[0001] The present invention belongs to the technical field of anti-seepage agents, and particularly relates to an anti-seepage additive for inkjet printing, a synthesis method thereof, and an anti-seepage process. Background Art

[0002] In the field of printed circuit board manufacturing, after the PCB circuit is fabricated, solder mask ink needs to be printed. The solder mask ink has three main functions. First, it covers the copper circuit and copper surface to prevent short circuits during wave soldering. Second, it acts as a protective layer to prevent the erosion and oxidation of the circuit by factors such as moisture, thereby affecting the electrical performance. Third, it acts as an insulating medium between copper conductors to improve insulation reliability.

[0003] The existing solder mask processes are mainly as follows: copper surface roughening, ink printing, pre-curing, exposure, development, and post-curing. This process has the following deficiencies: (1) The traditional solder mask process uses a subtractive process, and the ink contains organic solvents. Therefore, a large amount of waste water, waste liquid, and waste gas are discharged during the production process, and the environmental protection problem is prominent. (2) The traditional solder mask ink process takes a long time, and the process and upstream and downstream cannot achieve continuous production, making large-scale manufacturing difficult. (3) It is necessary to replace the screen or film according to the circuit image, and at the same time, the process requires a lot of equipment and consumes a large amount of energy, which is not conducive to reducing production costs.

[0004] In response to the above problems, the solder mask inkjet printing technology has emerged. Compared with the traditional solder mask process, the solder mask inkjet printing technology has a simple process, which only includes pre-treatment, inkjet printing, and curing. The production process takes a short time, consumes less energy, and generates less waste liquid, waste gas, and waste water, taking into account both economic and environmental benefits. In recent years, after continuous optimization and improvement, solder mask inkjet printing equipment and ink have gradually become marketable. However, there are still some problems at present. The surface tension of the inkjet printing ink is low. When the ink is sprayed on the surface of the substrate, the ink will spontaneously spread, thereby affecting the inkjet printing accuracy and subsequent processes.

[0005] The spread of the inkjet printing ink on the surface of the substrate is greatly affected by the surface energy of the substrate. An effective measure is to pre-treat the surface of the substrate to reduce the surface energy of the substrate. Therefore, it is particularly important to develop a new additive that can significantly reduce the surface energy of the substrate for the application and popularization of inkjet printing technology. Summary of the Invention

[0006] Aiming at the deficiencies of the prior art, the purpose of the present invention is to provide an anti-seepage additive for inkjet printing, a synthesis method thereof, and an anti-seepage process. After the substrate such as metal, resin, etc. is treated with the anti-seepage working fluid prepared with the anti-seepage additive provided in the present invention, a molecular film will be adsorbed on the surface, so that the surface energy of the substrate is decreased, thereby suppressing the spread of the inkjet printing ink on the surface of the substrate and improving the inkjet printing accuracy.

[0007] To achieve the object of the present invention, the following technical solutions are adopted in the present invention:

[0008] In a first aspect, the present invention provides an anti-seepage additive for inkjet printing. The synthesis raw materials of the anti-seepage additive for inkjet printing include compound A and compound B; compound A is a polysiloxane containing an amino group; compound B is a compound containing an acryloyloxy group or a compound containing an epoxy group.

[0009] The present invention aims to solve the problem that during the inkjet printing process, the printed ink is prone to spread on the surface of the substrate, resulting in poor printing accuracy. The spread of the printed ink on the surface of the substrate is greatly affected by the surface energy of the substrate. By pre-treating the surface of the substrate with anti-seepage treatment to reduce the surface energy of the substrate is an effective measure. In the present invention, compound A is a polysiloxane containing an amino group. The polysiloxane chain has the characteristics of low surface tension and high stability. The amino group in its molecular chain can be used as an adsorption site to physically or chemically adsorb to the surface of substrates such as metals, etc., thereby adsorbing to the surface of substrates such as metals, and significantly reducing the surface energy of the surface of substrates such as metals; the molecular structure of compound B has a hydrophilic group or generates a hydrophilic group after reacting with compound A. The molecular chain of the anti-seepage additive for inkjet printing generated after the reaction of chemical compound A and compound B can take into account the characteristics of both compound A and compound B, that is, it has the characteristic of low surface tension of compound A, and at the same time contains a hydrophilic group, improving the defect that compound A has poor dispersion in aqueous solution. Based on this, the surface of the substrate treated with the anti-seepage additive for inkjet printing has a significant inhibitory effect on the spread of the printed ink, and has the characteristics of good anti-seepage effect and good stability.

[0010] Preferably, the polysiloxane containing an amino group has the structure shown in formula I.

[0011]

[0012] In formula I, R1 and R3 each independently selected from any one of -NA2, -BNH2, -BNHA, -A, OA, -OH or -COOH, wherein A is an alkyl group having 1 to 5 carbon atoms (such as 2, 3 or 4), B is an alkylene group having 1 to 5 carbon atoms (such as 2, 3 or 4), and at least one of R1 and R3 is selected from any one of -NA2, -BNH2 or -BNHA.

[0013] In formula I, R2 is selected from -(R 1 O) x R 3 、-(R 1 O) x (R 2 O) y R 3 、-R 1 OCH2CHOHCH2R 4, any one of an alkyl group having 1 to 5 carbon atoms (e.g., 2, 3, or 4), an alkoxy group having 1 to 5 carbon atoms (e.g., 2, 3, or 4), or a hydroxyl group, where R 1 and R 2 each independently selected from an alkylene group having 1 to 5 carbon atoms (e.g., 2, 3, or 4), R 3 selected from hydrogen or an alkyl group having 1 to 5 carbon atoms (e.g., 2, 3, or 4), R 4 selected from -NHC2H4NH2 or -NHC3H6N(CH3)2, x is an integer from 1 to 20 (e.g., 2, 4, 6, 8, 10, 12, 14, 16, or 18, etc.), and y is an integer from 1 to 10 (e.g., 2, 3, 4, 5, 6, 7, 8, or 9, etc.).

[0014] In formula I, 10 < m + n ≤ 100, m and n are integers, for example, m + n = 20, m + n = 30, m + n = 40, m + n = 50, m + n = 60, m + n = 70, m + n = 80, or m + n = 90, etc., and n is an integer from 0 to 50 (e.g., 5, 10, 15, 20, 25, 30, 35, 40, or 45, etc.).

[0015] In the present invention, the surface energy of compound A is affected by the degree of polymerization. If the degree of polymerization is too small, it is not sufficient to significantly reduce the surface energy of the substrate after adsorbing on the substrate surface. Therefore, the degree of polymerization needs to be relatively high. However, if the degree of polymerization is too high, it will lead to poor dispersion ability in aqueous solution, and it is easy to have a relatively large diameter of the micro-droplet particles formed after dispersion or re-stratification after dispersion, resulting in a large number of dot-like residues or deteriorated performance on the substrate surface treated with the anti-seepage working fluid prepared with the anti-seepage additive for inkjet printing.

[0016] Preferably, in formula I, R1 and R3 each independently selected from any one of -N(CH3)2, -C2H4NH2, -C3H6NH2, -C4H8NHC2H5, or -CH3.

[0017] Preferably, in formula I, R2 is selected from -(C2H4O) x R 3 , -(C3H6O) x R 3 , -(C3H6O) x (C2H4O) y R 3 , -C3H6OCH2CHOHCH2NHC3H6N(CH3)2, -C3H6OCH2CHOHCH2NHC2H4NH2, -CH3, -OCH3, or -OH, R 3Each independently selected from any one of -H, -CH3 or -CH2CH3, wherein x is an integer from 10 to 20 (such as 11, 12, 13, 14, 15, 16, 17, 18 or 19, etc.), and y is an integer from 5 to 10 (such as 6, 7, 8 or 9, etc.).

[0018] Preferably, the acryloyloxy group-containing compound has the structure shown in Formula II-1 or Formula II-2.

[0019]

[0020] In Formula II-1 and Formula II-2, each R4 is independently selected from hydrogen, a substituted or unsubstituted alkyl group having 1 to 12 carbon atoms (such as 2, 4, 6, 8 or 10, etc.), a substituted or unsubstituted furyl group, a substituted or unsubstituted morpholinyl group, a substituted or unsubstituted piperidinyl group, a group having the structure shown in Formula 1, a group having the structure shown in Formula 2, a group having the structure shown in Formula 3 or a group having the structure shown in Formula 4.

[0021]

[0022] In Formula 1, Formula 2, Formula 3 and Formula 4, R 5 Each independently selected from an alkylene group having 1 to 5 carbon atoms (such as 2, 3 or 4, etc.), R 6 Selected from any one of hydrogen, an alkyl group having 1 to 5 carbon atoms (such as 2, 3 or 4, etc.) or benzyl, R 7 Selected from any one of an alkyl group having 1 to 5 carbon atoms (such as 2, 3 or 4, etc.) or benzyl, and q is an integer from 1 to 8 (such as 2, 3, 4, 5, 6 or 7, etc.).

[0023] The substituents of the substituted R4 are selected from any one or at least two combinations of a hydroxyl group, a halogen, an alkyl group having 1 to 12 carbon atoms (such as 2, 4, 6, 8 or 10, etc.) or an aryl group having 6 to 10 carbon atoms (such as 7, 8 or 9, etc.).

[0024] Preferably, in Formula II-1 and Formula II-2, each R4 is independently selected from -H, -(CH2) a CH3, -(CH2) a CH2OH, -(CH2) a CHOHCH3, -(C2H4O) q R 6 、-(CH2)2N + (CH3)2R 7 Cl - 、-(CH2)2PO4 - (CH2)2N + (CH3)3、-(CH2)2N+ (CH3)2(CH2)3SO3 - 、-(CH2) b C d F 2d+1 、-(CH2) b C d F 2d H, furyl, morpholinyl or piperidinyl, where a are each independently an integer from 0 to 10 (such as 1, 2, 3, 4, 5, 6, 7, 8 or 9, etc.), q are each independently an integer from 1 to 8 (such as 2, 3, 4, 5, 6 or 7, etc.), d are each independently an integer from 1 to 10 (such as 2, 3, 4, 5, 6, 7, 8 or 9, etc.), R 6 is selected from any one of hydrogen, an alkyl group having 1 to 5 carbon atoms (such as 2, 3 or 4, etc.) or benzyl, R 7 is selected from any one of an alkyl group having 1 to 5 carbon atoms (such as 2, 3 or 4, etc.) or benzyl.

[0025] Preferably, the R4 is selected from -(C2H4O) q R 6 、-(CH2)2N + (CH3)2R 7 Cl - 、-(CH2)2PO4 - (CH2)2N + (CH3)3 or -(CH2)2N + (CH3)2(CH2)3SO3 - any one of them.

[0026] Preferably, the acryloyloxy group-containing compound is selected from any one or a combination of at least two of the following compounds:

[0027]

[0028]

[0029] Preferably, the epoxy group-containing compound has any one of the structures shown in Formula III-1, Formula III-2 or III-3.

[0030]

[0031] In Formula III-1, R5 is selected from any one of a substituted or unsubstituted alkyl group having 1 to 12 carbon atoms, a substituted or unsubstituted alkenyl group having 1 to 12 carbon atoms, a substituted or unsubstituted aryl group having 6 to 12 carbon atoms or a polyether group having the structure shown in Formula IV-1.

[0032]

[0033] In formula Ⅳ-1, R 8 is an alkylene group having 1 to 5 carbon atoms, R 9 is an alkyl group having 1 to 5 carbon atoms, and f is an integer from 1 to 10.

[0034] In formula Ⅲ-2, R6 is selected from any one of a substituted or unsubstituted alkylene group having 1 to 12 carbon atoms, a substituted or unsubstituted alkenylene group having 1 to 12 carbon atoms, a substituted or unsubstituted arylene group having 6 to 12 carbon atoms, and a polyether group having the structure shown in formula Ⅳ-2.

[0035]

[0036] In formula Ⅳ-2, R 10 is an alkylene group having 1 to 5 carbon atoms, and s is an integer from 1 to 10.

[0037] The substituents in R5 and R6 are each independently selected from any one or at least two combinations of an alkyl group having 1 to 5 carbon atoms, an alkenyl group having 1 to 5 carbon atoms, or an aryl group having 6 to 10 carbon atoms.

[0038] In formula Ⅲ-3, each R7 is independently selected from an alkyl group having 1 to 12 carbon atoms.

[0039] Preferably, the compound containing an epoxy group is selected from any one or at least two combinations of the following compounds:

[0040]

[0041]

[0042] In the present invention, the compound B is preferably a compound having a hydrophilic structure in its molecular structure. For example, the compound B is preferably a compound having the structure shown in formula Ⅱ-1 or formula Ⅱ-2, wherein each R4 is independently selected from -(C2H4O) q R 6 、-(CH2)2N + (CH3)2R 7 Cl - 、-(CH2)2PO4 - (CH2)2N + (CH3)3、-(CH2)2N + (CH3)2(CH2)3SO3 - ; The compound B is preferably a compound having the structure shown in formula Ⅲ-3, which contains -CH2N + (R7)3Cl -The group is because the reactant A is an amino-containing polysiloxane, and its main chain is polysiloxane, which has poor dispersion ability in water. By reacting with the compound B with a hydrophilic structure, its dispersion ability in the aqueous solution can be improved, and the performance stability of the anti-seepage additive for inkjet printing can be enhanced. In addition, when the hydrophilic group in the molecule of the reactant B is a quaternary ammonium group, since the quaternary ammonium group can have a better adsorption effect with substrates such as metals, when the reactant B reacts with the reactant A, the quaternary ammonium group is grafted onto the polysiloxane chain, which can increase the density of active adsorption groups on the anti-seepage additive for inkjet printing and enhance the adsorption ability of the anti-seepage additive for inkjet printing on the surface of substrates such as metals (such as copper), thereby improving the anti-seepage effect of the substrates such as metals on the printed ink.

[0043] Preferably, the molar ratio of the compound A to the compound B is 1:(1.1 - 4.5), such as 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, etc.

[0044] In a second aspect, the present invention provides a synthesis method of the anti-seepage additive for inkjet printing as described in the first aspect, characterized in that the synthesis method comprises the following steps:

[0045] (1) Dissolve the compound A in a solvent to obtain a solution A.

[0046] (2) Dissolve the compound B in a solvent to obtain a solution B.

[0047] (3) Mix the solution A and the solution B, and react to obtain the anti-seepage additive for inkjet printing.

[0048] Among them, steps (1) and (2) are carried out step by step without a specific order, or simultaneously.

[0049] Preferably, the solvents in steps (1) and (2) independently include alcohols with 1 - 4 carbon atoms.

[0050] Preferably, the alcohol with 1 - 4 carbon atoms includes any one or a combination of at least two of methanol, ethanol, propanol, isopropanol or butanol.

[0051] Preferably, the mass ratio of the compound A to the solvent in step (1) is 1:(0.3 - 8), such as 1:1, 1:2, 1:3, 1:4, 1:5, 1:6 or 1:7, etc.

[0052] Preferably, the mass ratio of the compound B to the solvent in step (2) is 1:(0.3 - 8), such as 1:1, 1:2, 1:3, 1:4, 1:5, 1:6 or 1:7, etc.

[0053] Preferably, step (3) includes the following steps: under the atmosphere of nitrogen protection, stir and heat solution B, dropwise add solution A, react, and perform vacuum distillation to obtain the anti-seepage additive for inkjet printing.

[0054] In the present invention, step (3) removes the solvent and unreacted reactants by vacuum distillation.

[0055] Preferably, the rotation speed of the stirring in step (3) is 200 - 500 r / min, such as 230 r / min, 260 r / min, 290 r / min, 320 r / min, 350 r / min, 380 r / min, 410 r / min, 440 r / min or 470 r / min, etc.

[0056] Preferably, the heating in step (3) is to heat to 30 - 100 °C, such as 40 °C, 50 °C, 60 °C, 70 °C, 80 °C or 90 °C, etc.

[0057] Preferably, the time for dropwise adding solution A in step (3) is 1 - 4 h, such as 1.3 h, 1.6 h, 1.9 h, 2.2 h, 2.5 h, 2.8 h, 3.1 h, 3.4 h or 3.7 h, etc.

[0058] Preferably, the reaction temperature in step (3) is 30 - 100 °C (such as 40 °C, 50 °C, 60 °C, 70 °C, 80 °C or 90 °C, etc.), and the reaction time is 7 - 24 h (such as 9 h, 11 h, 13 h, 15 h, 17 h, 19 h, 21 h or 23 h, etc.).

[0059] In the third aspect, the present invention provides an anti-seepage process, and the anti-seepage process includes the following process:

[0060] (a) Prepare an anti-seepage agent by using the anti-seepage additive for inkjet printing as described in the first aspect.

[0061] (b) Prepare an anti-seepage working solution from the anti-seepage agent obtained in step (a).

[0062] (c) Spray the surface of the substrate with the anti-seepage working solution obtained in step (b).

[0063] (d) Wash and dry the substrate to complete the anti-seepage process.

[0064] Preferably, process (a) includes the following steps: mix the anti-seepage additive for inkjet printing as described in the first aspect with an organic solvent, stir and dissolve, dilute with water, adjust the pH with an acid, and make up the volume to obtain the anti-seepage agent.

[0065] Preferably, the concentration of the anti-seepage additive for inkjet printing in the anti-seepage agent in process (a) is 2.5 - 50 g / L, such as 5 g / L, 10 g / L, 15 g / L, 20 g / L, 25 g / L, 30 g / L, 35 g / L, 40 g / L or 45 g / L, etc.

[0066] Preferably, the concentration of the organic solvent in the anti-seepage agent in process (a) is 100 - 500 g / L, such as 150 g / L, 200 g / L, 250 g / L, 300 g / L, 350 g / L, 400 g / L or 450 g / L, etc.

[0067] Exemplarily, the organic solvent includes any one or a combination of at least two of organic solvents such as diethylene glycol, diethylene glycol monobutyl ether, diethylene glycol monohexyl ether, diethylene glycol monophenyl ether, ethylene glycol monoisopropyl ether or tripropylene glycol.

[0068] Preferably, the acid includes organic acid and / or inorganic acid.

[0069] Preferably, the acid includes any one or a combination of at least two of formic acid, acetic acid, phosphoric acid, boric acid, hydrochloric acid or sulfuric acid.

[0070] Preferably, the pH of the anti-seepage agent is 5.0 - 7.0, such as 5.2, 5.4, 5.6, 5.8, 6.0, 6.2, 6.4, 6.6 or 6.8, etc.

[0071] Preferably, process (b) includes the following steps: diluting the anti-seepage agent prepared in process (a) with water to obtain an anti-seepage working solution.

[0072] Preferably, the concentration of the anti-seepage agent in the anti-seepage working solution is 20 - 60 mL / L, such as 25 mL / L, 30 mL / L, 35 mL / L, 40 mL / L, 45 mL / L, 50 mL / L or 55 mL / L, etc.

[0073] Preferably, the substrate is a super-roughened board.

[0074] In the present invention, the super-roughened board means a copper clad laminate after super-roughening treatment. The super-roughening treatment can be carried out by methods well known in the art and will not be elaborated here.

[0075] Preferably, the spraying treatment in process (c) is continuous spraying treatment.

[0076] In the present invention, the process parameters of the spraying treatment in process (c) also have a certain influence on the anti-seepage effect.

[0077] Preferably, the temperature of the spraying treatment is 20 - 30 °C, such as 21 °C, 22 °C, 23 °C, 24 °C, 25 °C, 26 °C, 27 °C, 28 °C or 29 °C, etc.

[0078] In the present invention, the temperature of the continuous spraying treatment is preferably 20-30 °C. If the temperature is too low, the anti-seepage additive components for inkjet printing in the anti-seepage working fluid are likely to precipitate, resulting in a poor anti-seepage effect. If the temperature is too high, the volatilization rate of the organic solvent in the anti-seepage working fluid becomes too fast, which is not conducive to the stable operation of the anti-seepage working fluid.

[0079] Preferably, the spraying pressure of the continuous spraying treatment is 1-2.5 kg / cm 2 , such as 1.2 kg / cm 2 , 1.4 kg / cm 2 , 1.6 kg / cm 2 , 1.8 kg / cm 2 , 2.0 kg / cm 2 , 2.2 kg / cm 2 or 2.4 kg / cm 2 etc., and more preferably 1-2 kg / cm 2 .

[0080] In the present invention, the spraying pressure of the continuous spraying treatment is preferably 1-2.5 kg / cm 2 , if the pressure is too low, the contact between the anti-seepage working fluid and the substrate surface is insufficient, resulting in uneven adsorption of the anti-seepage additive for inkjet printing on the substrate surface, and there may be a phenomenon of poor local anti-seepage effect on the substrate surface. If the pressure is too high, the load on the circulation pump increases, shortening the service life of the circulation pump.

[0081] Preferably, the time of the continuous spraying treatment is 20-80 s, such as 25 s, 30 s, 35 s, 40 s, 45 s, 50 s, 55 s, 60 s, 65 s, 70 s or 75 s, etc.

[0082] In the present invention, the time of the continuous spraying treatment is preferably 20-80 s. If the time is too short, the adsorption of the anti-seepage additive for inkjet printing on the substrate surface is insufficient, resulting in a poor anti-seepage effect. If the spraying treatment time is too long, the production efficiency is reduced.

[0083] Compared with the prior art, the present invention has the following beneficial effects:

[0084] After the substrate surface is treated with the anti-seepage working fluid prepared from the anti-seepage additive for inkjet printing in the present invention, the surface energy of the substrate can be reduced, and thus the spontaneous diffusion of the inkjet ink on the substrate surface can be effectively inhibited. The anti-seepage effect is good, which helps to improve the inkjet printing accuracy. Description of the Drawings

[0085] Figure 1 Infrared spectra of Compound A, Compound B and the anti-seepage additive for inkjet printing in Example 1;

[0086] Figure 2 Infrared spectra of Compound A, Compound B, and the anti-seepage additive for inkjet printing in Example 2;

[0087] Figure 3 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 1 against the inkjet ink;

[0088] Figure 4 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 2 against the inkjet ink;

[0089] Figure 5 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 3 against the inkjet ink;

[0090] Figure 6 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 6 against the inkjet ink;

[0091] Figure 7 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 9 against the inkjet ink;

[0092] Figure 8 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 12 against the inkjet ink;

[0093] Figure 9 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 13 against the inkjet ink;

[0094] Figure 10 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Application Example 14 against the inkjet ink;

[0095] Figure 11 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Comparative Application Example 1 against the inkjet ink;

[0096] Figure 12 Anti-seepage effect diagram of the super-roughened plate treated with the anti-seepage working fluid prepared in Comparative Application Example 2 against the inkjet ink;

[0097] Figure 13 When the anti-seepage agent provided in Example 1 was subjected to the aging resistance test, the anti-seepage effect diagram of the inkjet ink after treating the super-roughened plate with 1 L of the anti-seepage working fluid continuously for 5 m 2 of the super-roughened plate and then treating another super-roughened plate;

[0098] Figure 14 When the anti-seepage agent provided in Example 1 was subjected to the aging resistance test, the anti-seepage effect diagram of the inkjet ink after treating the super-roughened plate with 1 L of the anti-seepage working fluid continuously for 10 m 2Effect diagram of anti-seepage of inkjet printing ink after reprocessing the super-roughened plate and then super-roughening the plate. Detailed implementation manners

[0099] The technical solutions of the present invention will be further described below through specific implementation manners. Those skilled in the art should understand that the embodiments are only for helping to understand the present invention and should not be regarded as specific limitations on the present invention.

[0100] Embodiment 1

[0101] This embodiment provides an anti-seepage additive for inkjet printing, its synthesis method and an anti-seepage agent. The synthesis raw materials of the anti-seepage additive for inkjet printing include compound A and compound B;

[0102] Compound A has the structure shown in Formula I below:

[0103]

[0104] In Formula I, both R1 and R3 are selected from -C3H6NH2, R2 is selected from -CH3, m = 6, n = 6, and m + n = 12;

[0105] Compound B has the structure shown in the following formula:

[0106]

[0107] The molar ratio of compound A to compound B is 1:2.

[0108] The synthesis method of the anti-seepage additive for inkjet printing includes the following steps:

[0109] (1) Dissolve 22.7 g of compound A in 25 g of isopropanol to obtain solution A;

[0110] (2) Dissolve 7.8 g of compound B in 10 g of isopropanol to obtain solution B;

[0111] (3) Under the atmosphere of nitrogen protection, stir and heat solution B to 50 °C, the stirring speed is 500 r / min, then drop solution A into solution B, finish dropping in 1 h, and then continue to react for 24 h. After the reaction ends, remove isopropanol and unreacted reactants by vacuum distillation to obtain the anti-seepage additive for inkjet printing.

[0112] The anti-seepage agent includes the above anti-seepage additive for inkjet printing, an organic solvent (diethylene glycol monobutyl ether), hydrochloric acid (concentration of 1 mol / L), and deionized water; the concentration of the anti-seepage additive for inkjet printing in the anti-seepage agent is 2.5 g / L, the concentration of the organic solvent is 100 g / L, and the pH of the anti-seepage agent is 5.0.

[0113] The preparation method of the anti-seepage agent comprises the following steps: adding the formulated amount of organic solvent into a reaction kettle, then adding the above anti-seepage additive for inkjet printing according to the formulated amount, fully stirring and dissolving, diluting with deionized water, adjusting the pH with hydrochloric acid, and making up the volume to obtain the anti-seepage agent.

[0114] Example 2

[0115] This example provides an anti-seepage additive for inkjet printing, its synthesis method and an anti-seepage agent. The synthesis raw materials of the anti-seepage additive for inkjet printing include compound A and compound B;

[0116] Compound A has the structure shown in Formula I as follows:

[0117]

[0118] In Formula I, R1 is selected from -C3H6NH2, R2 is selected from -(C2H4O) 20 CH3, R3 is selected from -CH3, m = 24, n = 1, m + n = 25;

[0119] Compound B has the structure shown in Formula II-1 as follows:

[0120]

[0121] The molar ratio of compound A to compound B is 1:1.1.

[0122] The synthesis method of the anti-seepage additive for inkjet printing comprises the following steps:

[0123] (1) Dissolve 60 g of compound A in 20 g of isopropanol to obtain solution A;

[0124] (2) Dissolve 3.6 g of compound B in 10 g of isopropanol to obtain solution B;

[0125] (3) Under the atmosphere of nitrogen protection, stir and heat solution B to 90 °C, the stirring speed is 500 r / min, then drop solution A into solution B, finish dropping in 1 h, and then continue to react for 16 h. After the reaction is completed, remove isopropanol and unreacted reactants by vacuum distillation to obtain the anti-seepage additive for inkjet printing.

[0126] The anti-seepage agent comprises the above anti-seepage additive for inkjet printing, an organic solvent (diethylene glycol monobutyl ether), phosphoric acid and deionized water; the concentration of the anti-seepage additive for inkjet printing in the anti-seepage agent is 50 g / L, the concentration of the organic solvent is 300 g / L, and the pH of the anti-seepage agent is 6.0.

[0127] The synthesis method of the anti-seepage agent includes the following steps: Add the formulated amount of organic solvent into the reaction kettle, then add the above-mentioned anti-seepage additive for inkjet printing according to the formulated amount. After fully stirring and dissolving, add deionized water for dilution and adjust the pH with phosphoric acid, and make up the volume to obtain the anti-seepage agent.

[0128] Example 3

[0129] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 is only the molecular structure and mass of compound B. Compound B has the structure shown in the following formula:

[0130]

[0131] In the synthesis method of the anti-seepage additive for inkjet printing, the mass of compound B is adjusted to 11.2 g, so that the molar ratio of compound A to compound B is 1:2.

[0132] Other conditions are the same as those in Example 1.

[0133] Example 4

[0134] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 is only the molecular structure and mass of compound B. Compound B has the structure shown in the following formula:

[0135]

[0136] In the synthesis method of the anti-seepage additive for inkjet printing, the mass of compound B is adjusted to 6.1 g, so that the molar ratio of compound A to compound B is 1:2.

[0137] Other conditions are the same as those in Example 1.

[0138] Example 5

[0139] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 is only that in the synthesis method of the anti-seepage additive for inkjet printing, the mass of compound B is adjusted to 15.6 g, so that the molar ratio of compound A to compound B is 1:4; other conditions are the same as those in Example 1.

[0140] Example 6

[0141] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 is only the molecular weight of compound A and the mass of compound B. Compound A has the structure shown in the following formula Ⅰ,

[0142]

[0143] In Formula I, both R1 and R3 are selected from -C3H6NH2, R2 is selected from -CH3, m = 39, n = 39, m + n = 78. In the preparation method of the anti-seepage additive for inkjet printing, the mass of Compound B is adjusted to 1.47 g, and the molar ratio of Compound A to Compound B is 1:2; other conditions are the same as those in Example 1.

[0144] Example 7

[0145] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 lies only in the molecular structure of Compound A and the mass of Compound B. Compound A has the structure shown in Formula I below.

[0146]

[0147] In Formula I, R1 is selected from -C3H6NH2, R2 is selected from -CH3, R3 is selected from -CH3, m = 6, n = 6, m + n = 12. In the preparation method of the anti-seepage additive for inkjet printing, the mass of Compound B is adjusted to 8.1 g, and the molar ratio of Compound A to Compound B is 1:2; other conditions are the same as those in Example 1.

[0148] Example 8

[0149] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 lies only in that the concentration of the anti-seepage additive for inkjet printing in the anti-seepage agent is adjusted to 25 g / L, and other conditions are the same as those in Example 1.

[0150] Example 9

[0151] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 lies only in that the pH of the anti-seepage agent is 7.0, and other conditions are the same as those in Example 1.

[0152] Example 10

[0153] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 lies only in that the concentration of the organic solvent in the anti-seepage agent is adjusted to 500 g / L, and other conditions are the same as those in Example 1.

[0154] Example 11

[0155] This example provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Example 1 lies only in that the organic solvent (diethylene glycol monobutyl ether) is replaced with the same mass of organic solvent (ethylene glycol propyl ether), and other conditions are the same as those in Example 1.

[0156] Example 12

[0157] This embodiment provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Embodiment 1 is only that Compound A has the structure shown in Formula I as follows:

[0158]

[0159] In Formula I, both R1 and R3 are selected from -C3H6NH2, R2 is selected from -CH3, m = 3, n = 2, m + n = 5; in the preparation method of the anti-seepage additive for inkjet printing, step (1) is adjusted to dissolve 12.3 g of Compound A in 13.5 g of isopropanol to obtain Solution A; the molar ratio of Compound A to Compound B is 1:2; other conditions are the same as those in Embodiment 1.

[0160] Embodiment 13

[0161] This embodiment provides an anti-seepage additive for inkjet printing, its synthesis method and anti-seepage agent. The difference from Embodiment 1 is only that Compound A has the structure shown in Formula I as follows,

[0162]

[0163] In Formula I, both R1 and R3 are selected from -C3H6NH2, R2 is selected from -CH3, m = 75, n = 75, m + n = 150; in the preparation method of the anti-seepage additive for inkjet printing, step (1) is adjusted to dissolve 227 g of Compound A in 250 g of isopropanol to obtain Solution A; the molar ratio of Compound A to Compound B is 1:2; other conditions are the same as those in Embodiment 1.

[0164] Other conditions are the same as those in Embodiment 1.

[0165] Comparative Example 1

[0166] This comparative example provides an anti-seepage agent. The difference from Embodiment 1 is only that the anti-seepage additive for inkjet printing is not added to the anti-seepage agent, and other conditions are the same as those in Embodiment 1.

[0167] Comparative Example 2

[0168] This comparative example provides an anti-seepage additive for inkjet printing and an anti-seepage agent. The difference from Embodiment 1 is only that the anti-seepage additive for inkjet printing has the structure shown in Formula V as follows:

[0169]

[0170] Other conditions are the same as those in Embodiment 1.

[0171] Application Example 1

[0172] This application example provides an anti-seepage process, and the anti-seepage method includes the following steps:

[0173] (a) Mix the anti-seepage agent provided in Example 1 with deionized water to prepare an anti-seepage working fluid. The concentration of the anti-seepage agent in the anti-seepage working fluid is 60 mL / L, and the temperature of the anti-seepage working fluid is 30 °C;

[0174] (b) Place the super-roughened plate in a spray tank and perform anti-seepage treatment with the anti-seepage working fluid prepared in step (a). The spray pressure of the spray is 2.5 kg / cm 2 , the treatment time of the spray is 60 s, and then it is washed with deionized water and dried to obtain the super-roughened plate treated with the anti-seepage working fluid.

[0175] Application Examples 2 to 13

[0176] Application Examples 2 to 13 respectively provide an anti-seepage process, and the difference from Application Example 1 is only that the anti-seepage agent provided in Example 1 is respectively replaced with the anti-seepage agents provided in Examples 2 to 13 with the same mass, and other conditions are the same as those in Application Example 1.

[0177] Application Example 14

[0178] This application example provides an anti-seepage process, and the anti-seepage method includes the following steps:

[0179] (a) Mix the anti-seepage agent provided in Example 1 with deionized water to prepare an anti-seepage working fluid. The concentration of the anti-seepage agent in the anti-seepage working fluid is 20 mL / L, and the temperature of the anti-seepage working fluid is 20 °C;

[0180] (b) Place the super-roughened plate in a spray tank and perform anti-seepage treatment with the anti-seepage working fluid prepared in step (a). The spray pressure of the spray is 1 kg / cm 2 , the treatment time of the spray is 20 s, and then it is washed with deionized water and dried to obtain the super-roughened plate treated with the anti-seepage working fluid.

[0181] Comparative Application Examples 1 to 2

[0182] They respectively provide an anti-seepage process, and the difference from Application Example 1 is only that the anti-seepage agent provided in Example 1 is respectively replaced with the anti-seepage agents provided in Comparative Examples 1 to 2 with the same mass, and other conditions are the same as those in Application Example 1.

[0183] Perform the following performance tests on the super-roughened plates treated with the anti-seepage working fluids prepared in the above Application Examples 1 to 14 and Comparative Application Examples 1 to 2.

[0184] (1) Anti-seepage effect test: Use a dropper to drop the same type of inkjet ink on the surface of the super-roughened board treated with the anti-seepage working fluid respectively, and observe the diffusion of the inkjet ink. If the inkjet ink does not diffuse, the anti-seepage effect is considered good; if the inkjet ink diffuses slightly, the anti-seepage effect is considered average; if the inkjet ink diffuses in a large area, the anti-seepage effect is considered poor.

[0185] (2) Anti-seepage agent residue test: Electroplate copper on the super-roughened board treated with the anti-seepage working fluid, clean and dry it after electroplating, and then perform reflow soldering 20 times. Observe the delamination situation between the copper plating layer and the super-roughened board treated with the anti-seepage working fluid. If delamination or board explosion occurs, it is considered unqualified, otherwise it is considered qualified.

[0186] (3) Adhesion test: Spray the same type of inkjet ink (spraying thickness is 25μm) on the surface of the super-roughened board through an inkjet printer, and then perform pre-curing (80°C, 1h), photo-curing (500mJ / cm 2 ) and thermal curing (150°C, 1h) in sequence to form ink droplets. Use a scalpel to make two incisions with a spacing of 1 cm on the surface of the cured ink droplets, then soak them in 6N hydrochloric acid for 10 minutes, wash, dry, and use 3M 600 series tape to adhere to the ink surface for peeling treatment to evaluate the adhesion strength of the solder mask ink on the copper clad laminate. If the ink droplets do not fall off after 3 consecutive pull-offs, it is considered qualified, otherwise it is considered unqualified.

[0187] (4) Thermal reliability test: Spray the same type of inkjet ink (spraying thickness is 25μm) on the surface of the super-roughened board through an inkjet printer, and then perform pre-curing (80°C, 1h), photo-curing (500mJ / cm 2 ) and thermal curing (150°C, 1h) in sequence. After the inkjet ink is completely cured, perform a thermal shock test on it. Specifically, perform solder dipping treatment on it, the temperature of solder dipping is 288°C, and the number of times is 6 times. If the ink droplets formed by the curing of the inkjet ink do not fall off during the 6 tests, it is qualified, otherwise it is considered unqualified.

[0188] The test results are shown in Table 1 below.

[0189] Table 1

[0190] Seepage prevention effect Seepage prevention agent residue Bonding strength Thermal reliability Application Example 1 Good Qualified Qualified Qualified Application Example 2 Good Qualified Qualified Qualified Application Example 3 Good Qualified Qualified Qualified Application Example 4 Good Qualified Qualified Qualified Application Example 5 Good Qualified Qualified Qualified Application Example 6 Good Qualified Qualified Qualified Application Example 7 Good Qualified Qualified Qualified Application Example 8 Good Qualified Qualified Qualified Application Example 9 Good Qualified Qualified Qualified Application Example 10 Good Qualified Qualified Qualified Application Example 11 Good Qualified Qualified Qualified Application Example 12 Average Qualified Qualified Qualified Application Example 13 Average Unqualified Unqualified Unqualified Application Example 14 Good Qualified Qualified Qualified Comparative Application Example 1 Poor — — — Comparative Application Example 2 Poor — — —

[0191] In Table 1, "-" represents that this test item was not carried out.

[0192] The anti-seepage agents provided in the above Examples 1-13 and Comparative Examples 1-2 were tested as follows.

[0193] (1) Storage stability: The anti-seepage agent is stored at -5°C and 40°C for 10 days, and the appearance of the anti-seepage agent is observed to see if there are any undesirable phenomena such as oil floating, stratification, turbidity, etc. If there are any undesirable phenomena, it is considered unqualified, otherwise it is qualified.

[0194] (2) Aging resistance test: The anti-seepage agent and deionized water were mixed to form an anti-seepage working solution. The concentration of the anti-seepage agent in the anti-seepage working solution was 40 mL / L. 5 L of the anti-seepage working solution was placed in a sprayer and then heated to 25°C. After heating, the ultra-roughened board was sprayed at a spray pressure of 1 kg / cm 2 The spraying time is 40s; after the anti-seepage working solution is consumed, the anti-seepage agent is added to the spray tank manually, and the amount of each addition is 5mL / (m 2 ·L), and the pH of the anti-seepage working fluid is monitored online by an online pH detector to control the pH of the anti-seepage working fluid within the range of 5 to 7. Each liter of anti-seepage working fluid continuously treats 5m 2 After the super-roughened board, evaluate whether the anti-seepage effect of the inkjet printing ink can be maintained when the super-roughened board is reprocessed. If it can be maintained, it is qualified, if not, it is unqualified.

[0195] The test results are shown in Table 2 below.

[0196] Table 2

[0197]

[0198] In Table 2, “—” means that the test was not conducted.

[0199] It can be seen from the contents of Table 1 and Table 2 that the anti-seepage agent prepared with the anti-seepage additive for inkjet printing prepared in Examples 1 to 13 has good storage stability and good aging resistance. The ultra-roughened board treated with the prepared anti-seepage working fluid has good stability. The anti-seepage treatment does not affect the bonding strength between the inkjet printing ink and the copper surface of the ultra-roughened board, and has no negative impact on thermal reliability.

[0200] Depend on Figure 1 It can be seen that compound A (denoted as A1) in Example 1 has a wave number of 788 cm -1 (Si-CH3, Si-CH2-), 1021~1088cm -1 (Si-O) and 1257cm -1 Four groups of vibration absorption peaks unique to the main chain of polysiloxane appear at (Si-CH3). Since the molecular weight of A1 is relatively large and the amino content is low, no -NH2 absorption peak appears in the infrared spectrum. Compound B (denoted as B1) in Example 1 is acryloyloxyethyl trimethylammonium chloride, which has a wave number of 951 cm -1 1188cm -1 ~1268cm-1 at 1481 cm -1 at 1636 cm -1 at 1726 cm -1 has characteristic absorption peaks, corresponding to the vibrational absorptions of C-N, C-O, C-H, C═C, and C═O bonds respectively; A1 and B1 can undergo a Michael addition reaction through the amino group and the double bond. After the reaction, the double bond disappears and the primary amine is converted into a secondary amine. The product of A1 and B1 (denoted as C1) has, in its infrared spectrum, the absorption peaks of the polysiloxane chain attributed to A1 (788 cm -1 , 1009 cm -1 , 1088 cm -1 , 1257 cm -1 ) and the C═O absorption peak of B1 (1739 cm -1 ), but the absorption peak of C═C (1636 cm -1 ) attributed to B1 disappears, indicating that A1 and B1 have successfully reacted to form a new substance C1, that is, the anti-seepage additive for inkjet printing prepared in Example 1.

[0201] It can be seen from Figure 2 that compound A (denoted as A2) in Example 2 has four groups of characteristic vibrational absorptions of the polysiloxane main chain at the wave numbers of 788 cm -1 (Si-CH3, Si-CH2-), 1012 - 1079 cm -1 (Si-O), and 1256 cm -1 (Si-CH3). Since A2 has a larger molecular weight and a lower amino group content, no -NH2 absorption peak and characteristic absorption peaks appear in the infrared spectrum; compound B (denoted as B2) in Example 2 is ethylene glycol diglycidyl ether and has strong absorption peaks at the wave numbers of 755 cm -1 , 851 cm -1 , 910 cm -1 and 1091 cm -1 , corresponding to the characteristic absorption peaks of the epoxy group and the C-O-C bond; A2 and B2 can undergo an addition reaction through the amino group and the epoxy group. After the reaction, the epoxy group ring-opens to form an alcohol and the primary amine is converted into a secondary amine. The product of A2 and B2 (denoted as C2) has, in its infrared spectrum, the absorption peaks of the polysiloxane chain attributed to A2 (786 cm -1 , 1009 cm -1 , 1082 cm -1 , 1260 cm -1 ), and the characteristic absorption peaks attributed to B2 disappear, indicating that A2 and B2 have successfully reacted to form a new substance C2, that is, the anti-seepage additive for inkjet printing prepared in Example 2.

[0202] From Application Examples 1, 2, 3, 6 and Comparative Application Example 1, it can be seen that when the prepared anti-seepage agent working solution contains the anti-seepage additive component for inkjet printing, the inkjet ink does not spread on the surface of the super-roughened plate after treatment. As Figures 3 - 6 shown, if the prepared anti-seepage agent working solution does not contain the anti-seepage additive component for inkjet printing, the inkjet ink significantly spreads on the surface of the super-roughened plate after treatment. As Figure 11 shown, this shows that the anti-seepage additive component has a significant impact on the anti-seepage effect, and further illustrates that the anti-seepage additive for inkjet printing provided by the present invention has excellent anti-seepage effect.

[0203] From Application Example 1 and Application Example 9, it can be seen that when the pH of the anti-seepage agent is in the range of 5.0 - 7.0, for the super-roughened plate treated with the prepared anti-seepage working solution, the inkjet ink does not spread on its surface. As Figure 3 and Figure 7 shown. Thus, it can be known that within this pH range, the anti-seepage additive for inkjet printing provided by the present invention has chemical stability, and thus the anti-seepage performance is stable.

[0204] From Application Example 1 and Application Example 14, it can be seen that when the concentration of the anti-seepage agent in the anti-seepage working solution is in the range of 20 - 60 mL / L, the spraying temperature is in the range of 20 - 30 °C, the spraying pressure is in the range of 1 - 2 kg / cm 2 range, and the spraying treatment time is in the range of 20 - 60 s, the inkjet ink does not spread on the surface of the super-roughened plate treated with the anti-seepage working solution. As Figure 3 and Figure 10 shown, indicating that under this anti-seepage process, the anti-seepage effect of the anti-seepage agent working solution is good.

[0205] Compared with Application Example 1, if the polymerization degree of Compound A is too small, the prepared anti-seepage working solution is used for the anti-seepage treatment of the super-roughened plate (Application Example 12), and the anti-seepage effect is as Figure 8 shown, and the inkjet ink undergoes a certain degree of diffusion, resulting in a decrease in the anti-seepage effect.

[0206] Compared with Application Example 1, if the polymerization degree of Compound A is too large, the prepared anti-seepage working solution is used for the anti-seepage treatment of the super-roughened plate (Application Example 13), and the anti-seepage effect is as Figure 9 shown, and the inkjet ink undergoes slight diffusion, resulting in a decrease in the anti-seepage effect; in addition, there is obvious material residue on the surface of the treated super-roughened plate, resulting in poor bonding force between the inkjet ink and the copper surface, and the cured inkjet ink falls off after thermal shock.

[0207] Compared with Application Example 1, if the anti-seepage additive for inkjet printing is hydroxy-terminated polydimethylsiloxane (Comparative Example 2), and there is no amino group in its molecular structure, the prepared anti-seepage working solution is used for the anti-seepage treatment of the super-roughened plate (Comparative Application Example 2), and the anti-seepage effect is as Figure 12As shown, the inkjet printing ink diffuses significantly on the treated copper surface, and the anti-seepage effect is significantly worse than that of Application Example 1 and equivalent to that of Comparative Application Example 1, indicating that the amino structure has a significant impact on the anti-seepage effect of the anti-seepage additive for inkjet printing. This is because when there is no amino group in the molecular structure of the anti-seepage additive, it is difficult to adsorb onto the copper surface and thus cannot play its role.

[0208] It can be seen from Figure 12 , 13 that when the anti-seepage agent provided in Example 1 is used for continuous anti-seepage treatment during the aging resistance test on ultra-roughened plates of 5m 2 / L and 10m 2 / L, good anti-seepage effects are maintained and the aging resistance is good.

[0209] In summary, the anti-seepage agent prepared from the anti-seepage additive for inkjet printing described in the present invention can effectively inhibit the spontaneous diffusion of the inkjet printing ink, has a good anti-seepage effect, good storage stability, good binding effect with the inkjet printing ink, and stable performance after aging.

[0210] The applicant declares that the present invention uses the above embodiments to illustrate the process method of the present invention, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. Those skilled in the art should understand that any improvement to the present invention, the equivalent replacement of the raw materials selected for the present invention, the addition of auxiliary components, and the selection of specific methods, etc., all fall within the protection scope and the disclosure scope of the present invention.

Claims

1. An anti-seepage additive for inkjet printing, characterized in that: The synthetic raw materials of the inkjet printing anti-seepage additive include compound A and compound B; the compound A is amino-containing polysiloxane; the compound B is an acryloxy-containing compound or an epoxy-containing compound.

2. The anti-seepage additive for inkjet printing according to claim 1, characterized in that: The amino-containing polysiloxane has a structure shown in Formula I; In Formula I, R1 and R3 are each independently selected from any one of -NA2, -BNH2, -BNHA, -A, OA, -OH or -COOH, wherein A is an alkyl group having 1 to 5 carbon atoms, B is an alkylene group having 1 to 5 carbon atoms, and at least one of R1 and R3 is selected from any one of -NA2, -BNH2 or -BNHA; In Formula I, R2 is selected from -(R 1 O) x R 3 、-(R 1 O) x (R 2 O) y R 3 , -R 1 OCH2CHOHCH2R 4 , any one of an alkyl group having 1 to 5 carbon atoms, an alkoxy group having 1 to 5 carbon atoms, or a hydroxyl group, wherein R 1 and R 2 are each independently selected from an alkylene group having 1 to 5 carbon atoms, R 3 is selected from hydrogen or an alkyl group having 1 to 5 carbon atoms, R 4 Selected from -NHC2H4NH2 or -NHC3H6N(CH3)2, x is an integer from 1 to 20, and y is an integer from 1 to 10; In formula I, 10<m+n≤100, m and n are integers, and n is an integer of 0-50.

3. The anti-seepage additive for inkjet printing according to claim 2, characterized in that: In the formula I, R1 and R3 are each independently selected from any one of -N(CH3)2, -C2H4NH2, -C3H6NH2, -C4H8NHC2H5 or -CH3; Preferably, in the formula I, R2 is selected from -(C2H4O) x R 3 、-(C3H6O) x R 3 、-(C3H6O) x (C2H4O) y R 3 , -C3H6OCH2CHOHCH2NHC3H6N(CH3)2, -C3H6OCH2CHOHCH2NHC2H4NH2, -CH3, -OCH3 or -OH, any one of R 3 Each is independently selected from any one of -H, -CH3 or -CH2CH3, wherein x is an integer of 10 to 20, and y is an integer of 5 to 10.

4. The anti-seepage additive for inkjet printing according to any one of claims 1 to 3, characterized in that: The compound containing an acryloyloxy group has a structure shown in Formula II-1 or Formula II-2; In formula II-1 and formula II-2, R4 is independently selected from any one of hydrogen, a substituted or unsubstituted alkyl group having 1 to 12 carbon atoms, a substituted or unsubstituted furyl group, a substituted or unsubstituted morpholinyl group, a substituted or unsubstituted piperidinyl group, a group having a structure represented by formula 1, a group having a structure represented by formula 2, a group having a structure represented by formula 3, or a group having a structure represented by formula 4; In formula 1, formula 2, formula 3 and formula 4, R 5 are each independently selected from an alkylene group having 1 to 5 carbon atoms, R 6 Each is independently selected from any one of hydrogen, an alkyl group having 1 to 5 carbon atoms, or a benzyl group, R 7 Any one selected from an alkyl group or a benzyl group having 1 to 5 carbon atoms, and q is an integer of 1 to 8; The substituent in R4 is selected from any one or a combination of at least two of hydroxyl, halogen, alkyl having 1 to 12 carbon atoms or aryl having 6 to 10 carbon atoms; Preferably, in Formula II-1 and Formula II-2, R4 is independently selected from -H, -(CH2) a CH3, -(CH2) a CH2OH, -(CH2) a CHOHCH3, -(C2H4O) q R 6 、-(CH2)2N + (CH3)2R 7 Cl - 、-(CH2)2PO4 - (CH2)2N + (CH3)3, -(CH2)2N + (CH3)2(CH2)3SO3 - 、-(CH2) b C d F 2d+1 、-(CH2) b C d F 2d H, furanyl, morpholinyl or piperidinyl, wherein a is each independently an integer of 0 to 10, q and b are each independently an integer of 1 to 8, d is each independently an integer of 1 to 10, and R 6 Each is independently selected from any one of hydrogen, an alkyl group having 1 to 5 carbon atoms, or a benzyl group, R 7 Any one selected from an alkyl group or a benzyl group having 1 to 5 carbon atoms; Preferably, the compound containing an acryloyloxy group is selected from any one or a combination of at least two of the following compounds:

5. The anti-seepage additive for inkjet printing according to any one of claims 1 to 4, characterized in that: The epoxy group-containing compound has any one of the structures shown in Formula III-1, Formula III-2 or Formula III-3; In formula III-1, R5 is selected from any one of a substituted or unsubstituted alkyl group having 1 to 12 carbon atoms, a substituted or unsubstituted alkenyl group having 1 to 12 carbon atoms, a substituted or unsubstituted aryl group having 6 to 12 carbon atoms, or a polyether group having the structure shown in formula IV-1; In Formula IV-1, R 8 is an alkylene group having 1 to 5 carbon atoms, R 9 is an alkyl group having 1 to 5 carbon atoms, and f is an integer of 1 to 10; In formula III-2, R6 is selected from any one of a substituted or unsubstituted alkylene group having 1 to 12 carbon atoms, a substituted or unsubstituted alkenylene group having 1 to 12 carbon atoms, a substituted or unsubstituted arylene group having 6 to 12 carbon atoms, and a polyether group having the structure shown in formula IV-2; In Formula IV-2, R 10 is an alkylene group having 1 to 5 carbon atoms, and s is an integer of 1 to 10; The substituents in R5 and R6 are each independently selected from any one or a combination of at least two of an alkyl group having 1 to 5 carbon atoms, an alkenyl group having 1 to 5 carbon atoms, or an aryl group having 6 to 10 carbon atoms; In formula III-3, R7 are each independently selected from an alkyl group having 1 to 12 carbon atoms; Preferably, the epoxy-containing compound is selected from any one or a combination of at least two of the following compounds: Preferably, the molar ratio of compound A to compound B is 1:(1.1-4.5).

6. A method for synthesizing the anti-seepage additive for inkjet printing according to any one of claims 1 to 5, characterized in that: The synthesis method comprises the following steps: (1) dissolving compound A in a solvent to obtain solution A; (2) dissolving compound B in a solvent to obtain solution B; (3) mixing solution A and solution B, reacting to obtain the anti-seepage additive for inkjet printing; Wherein, step (1) and step (2) are performed in no particular order, or are performed simultaneously.

7. The synthesis method according to claim 6, characterized in that The solvents in step (1) and step (2) each independently include an alcohol having 1 to 4 carbon atoms; Preferably, the alcohol having 1 to 4 carbon atoms includes any one of methanol, ethanol, propanol, isopropanol or butanol, or a combination of at least two thereof; Preferably, the mass ratio of compound A to solvent in step (1) is 1:(0.3-8); Preferably, the mass ratio of compound B to solvent in step (2) is 1:(0.3-8); Preferably, the step (3) comprises the following steps: stirring and heating the solution B under a nitrogen atmosphere, adding the solution A dropwise, reacting, and distilling under reduced pressure to obtain the inkjet printing anti-seepage additive; Preferably, the stirring speed in step (3) is 200 to 500 r / min; Preferably, the heating in step (3) is heating to 30-100° C. Preferably, the time for adding solution A in step (3) is 1 to 4 hours; Preferably, the reaction temperature in step (3) is 30 to 100° C., and the reaction time is 7 to 24 hours.

8. An anti-seepage process, characterized in that: The anti-seepage process includes the following steps: (a) preparing an anti-seepage agent using the anti-seepage additive for inkjet printing according to any one of claims 1 to 5; (b) preparing an anti-seepage working solution by preparing the anti-seepage agent obtained in step (a); (c) spraying the surface of the substrate with the anti-seepage working solution prepared in step (b); (d) washing and drying the substrate to complete the anti-seepage process.

9. The anti-seepage process according to claim 8, characterized in that: Process (a) comprises the following steps: mixing the anti-seepage additive for inkjet printing according to any one of claims 1 to 5 and an organic solvent, stirring to dissolve, diluting with water, adding acid to adjust the pH, and fixing the volume to obtain an anti-seepage agent; Preferably, the concentration of the inkjet printing anti-seepage additive in the anti-seepage agent of process (a) is 2.5 to 50 g / L; Preferably, the concentration of the organic solvent in the impermeable agent in process (a) is 100 to 500 g / L; Preferably, the acid comprises an organic acid and / or an inorganic acid; Preferably, the acid comprises any one or a combination of at least two of formic acid, acetic acid, phosphoric acid, boric acid, hydrochloric acid or sulfuric acid; Preferably, the pH of the anti-seepage agent is 5.0-7.

0.

10. The anti-seepage process according to claim 8 or 9, characterized in that: Process (b) comprises the following steps: diluting the anti-seepage agent obtained in process (a) with water to obtain an anti-seepage working solution; Preferably, the concentration of the anti-seepage agent in the anti-seepage working solution is 20 to 60 mL / L; Preferably, the spraying treatment in process (c) is a continuous spraying treatment; Preferably, the temperature of the spray treatment is 20-30°C; Preferably, the spraying pressure of the spraying treatment is 1 to 2.5 kg / cm 2 ; Preferably, the spraying treatment lasts for 20 to 80 seconds.