Preparation method of cold-resistant low-temperature printing ink

Abstract

The invention relates to a preparation method of cold-resistant low-temperature ink, and belongs to the technical field of ink. Adding polyurethane resin into the cold-resistant solvent, and stirring and mixing to form a uniform resin solution; adding a pigment and a fatty acid macrogol ester dispersant into the resin solution, stirring, and dispersing at a high speed to obtain a pigment dispersion liquid; sequentially adding a plasticizer, an organic silicon defoaming agent, an acrylate flatting agent, a cold-resistant synergist and a glycerol antifreezing agent into the pigment dispersion liquid, and stirring and mixing; the mixed printing ink is ground through a three-roller grinding machine; and filtering the ground printing ink by using a filter membrane, and filling the printing ink into a packaging container to obtain the cold-resistant low-temperature printing ink. The cold-resistant synergist is prepared from 2-ethynyl quinoline, ethynyl phenyl sulfide, diphenyl azide phosphate, cuprous bromide and N, N, N ', N' ', N' '-pentamethyldiethylenetriamine, and the ink prepared by the invention has good fluidity at low temperature, high drying speed and strong adhesive force.

Description

Technical Field

[0001] The invention relates to the technical field of ink, in particular to a method for preparing cold-resistant and low-temperature ink. Background Art

[0002] In cold regions or under special low-temperature working conditions, conventional inks often experience performance degradation. For example, the ink's viscosity increases significantly, resulting in poor fluidity and difficulty achieving uniform printing. Drying speed slows, impacting production efficiency. Furthermore, the ink's adhesion to the printed substrate decreases, making the printed pattern susceptible to peeling and fading.

[0003] While some low-temperature inks are currently available on the market, they suffer from limitations such as limited cold resistance, high costs, and complex manufacturing processes. Some low-temperature inks still cannot meet practical requirements in extremely cold conditions, and their preparation may require specialized equipment and complex operational procedures, hindering large-scale production and application. Therefore, developing a low-temperature ink with excellent cold resistance, low cost, and simple manufacturing processes is of great practical significance. Summary of the Invention

[0004] In order to solve the above problems, the present invention provides a method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0005] S1 premix:

[0006] Add 20-35 parts of polyurethane resin to 30-50 parts of cold-resistant solvent, and stir at room temperature at a stirring speed of 150-250 r / min for 30-60 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0007] S2 pigment dispersion:

[0008] Add 10-20 parts of pigment and 0.5-1.5 parts of fatty acid polyethylene glycol ester dispersant to the resin solution, increase the stirring speed to 300-500 r / min, and stir for 60-90 minutes; at the same time, use a high-speed disperser at a speed of 3000-5000 r / min to disperse the pigment at a speed of 3000-5000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0009] S3 Additive Mixing:

[0010] Add 3-8 parts of plasticizer, 0.5-1 part of silicone defoamer, 0.5-1 part of acrylate leveling agent, 0.1-1 part of cold resistance synergist, and 0.5-1 part of glycerol antifreeze to the pigment dispersion in sequence, and stir at a stirring speed of 200-300 r / min for 40-60 minutes to fully mix the additives;

[0011] S4 grinding and refining:

[0012] Grind the mixed ink through a three-roll mill for 2-4 times, controlling the fineness of the ink to be between 10-15 μm to improve the uniformity of the ink and the printing quality;

[0013] S5 filter packaging:

[0014] The ground ink is filtered using a filter membrane with a pore size of 5-10 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0015] The cold-resistant solvent is ethylene glycol ethyl ether or propylene glycol methyl ether.

[0016] The pigment is one of titanium dioxide, carbon black, phthalocyanine blue and quinacridone red.

[0017] The plasticizer is dioctyl sebacate or diisononyl adipate.

[0018] The preparation method of the cold-resistant synergist is:

[0019] T1: Add 13-26 parts of 2-ethynylquinoline and 1-3 parts of ethynylphenyl sulfide to 200-300 parts of N,N-dimethylformamide, and then add 27-34 parts of diphenylphosphoryl azide, 0.2-0.6 parts of cuprous bromide, and 0.4-0.8 parts of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture is stirred at 50-70°C and 200-250 rpm for 4-6 hours. The reaction progress is monitored by high performance liquid chromatography. The reaction is considered complete when the content of the azide compound no longer changes.

[0020] T2: After the reaction is completed, filter and then transfer the filtrate to a vacuum distillation apparatus, and perform vacuum distillation at a temperature of 70-80°C to remove excess N,N-dimethylformamide to obtain a cold resistance enhancer.

[0021] The functional groups in molecules such as diphenyl phosphate, quinoline, and phenyl sulfide cooperate with each other in various ways to improve the cold resistance of inks. The specific mechanisms are as follows:

[0022] The role of diphenyl phosphate functional groups

[0023] The flexibility and plasticizing effect of the ester group: The ester group (-COO-) in the diphenyl phosphate molecule has a certain degree of flexibility, acting like a "lubricant" between molecular chains. It can be inserted between polymer chains in the ink, weakening the forces between the chains and increasing the space for the chains to move. This allows the chains to move relatively easily even at low temperatures, thereby improving the ink's flexibility and cold resistance. At the same time, the ester group can form hydrogen bonds or van der Waals forces with the polar groups on the polymer chains, further regulating the interactions between the molecular chains and maintaining good performance at low temperatures.

[0024] The role of the quinoline functional group

[0025] The polarity of nitrogen atoms and intermolecular interactions: The nitrogen atoms in quinoline molecules have a high electronegativity, giving quinoline a certain degree of polarity. This polarity enables quinoline to bond with the polymer chains in the ink through polar interactions. Nitrogen atoms can form hydrogen bonds or other weaker chemical bonds with certain groups on the polymer chains, thereby changing the arrangement of the polymer chains, increasing the distance between the chains, weakening the interaction forces, and increasing the flexibility and mobility of the chains, thereby improving the cold resistance of the ink.

[0026] The role of phenyl sulfide functional group

[0027] Sulfur atom flexibility and molecular chain motion: The sulfur atoms in phenyl sulfide have a large atomic radius and a certain degree of flexibility. In ink systems, the flexibility of the sulfur atoms can drive the movement of surrounding polymer molecular segments, effectively introducing flexible segments into the molecular chain. This makes the molecular chain more susceptible to twisting and rotation at low temperatures, increasing its flexibility and thus improving the cold resistance of the ink.

[0028] The functional groups in molecules such as diphenyl phosphate, quinoline, and phenyl sulfide act on the polymer molecular chains in the ink from different aspects through their respective characteristics, which collectively play a role in weakening the forces between molecular chains, hindering crystallization, increasing the flexibility of molecular chains, and improving the stability of the system, thereby effectively improving the cold resistance of the ink. DETAILED DESCRIPTION

[0029] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the invention, the specific implementation methods, structures, features and effects of the present invention are described in detail below in combination with preferred embodiments.

[0030] After being placed in a -20°C environment for 24 hours, the following performance tests were performed:

[0031] 1. Fluidity test: Use the outflow cup method to test the outflow time of the ink;

[0032] 2. Drying speed test: record the time it takes for the ink surface to dry at -20°C;

[0033] 3. Adhesion test: Print the ink on polyethylene plastic film and use the tape sticking method to test the adhesion of the ink.

[0034] Example 1

[0035] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0036] S1 premix:

[0037] Add 20g of Baowei waterborne polyurethane resin 006 to 30g of cold-resistant solvent and stir at room temperature at a stirring speed of 150r / min for 30 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0038] S2 pigment dispersion:

[0039] Add 10 g of pigment and 0.5 g of fatty acid polyethylene glycol ester PEG400DL dispersant to the resin solution, increase the stirring speed to 300 / min, and stir for 60 minutes; at the same time, use a high-speed disperser at a speed of 3000 r / min to disperse the pigment at a speed of 3000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0040] S3 Additive Mixing:

[0041] To the pigment dispersion, 3 g of plasticizer, DF677 silicone defoamer, 0.5g BYK-358N acrylate leveling agent, 0.1g cold resistance synergist, 0.5g glycerol antifreeze, stir at a stirring speed of 200r / min for 40 minutes to fully mix the additives;

[0042] S4 grinding and refining:

[0043] The mixed ink is ground through a three-roll mill for 2 times, and the fineness of the ink is controlled at 15μm to improve the uniformity of the ink and the printing quality;

[0044] S5 filter packaging:

[0045] The ground ink is filtered using a filter membrane with a pore size of 10 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0046] The cold-resistant solvent is ethylene glycol ethyl ether.

[0047] The pigment is titanium dioxide.

[0048] The plasticizer is dioctyl sebacate.

[0049] The preparation method of the cold-resistant synergist is:

[0050] T1: 13 g of 2-ethynylquinoline and 1 g of ethynylphenyl sulfide were added to 200 g of N,N-dimethylformamide, followed by the addition of 27 g of diphenylphosphoryl azide, 0.2 g of cuprous bromide, and 0.4 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture was stirred at 50°C and 200 rpm for 4 hours. The reaction progress was monitored by high performance liquid chromatography. The reaction was considered complete when the content of the azide compound no longer changed.

[0051] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 70°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0052] Example 2

[0053] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0054] S1 premix:

[0055] Add 25g of Baowei waterborne polyurethane resin 006 to 35g of cold-resistant solvent and stir at a stirring speed of 200r / min at room temperature for 40 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0056] S2 pigment dispersion:

[0057] 13 g of pigment and 0.8 g of fatty acid polyethylene glycol ester PEG400DL dispersant were added to the resin solution, the stirring speed was increased to 350 r / min, and the mixture was stirred for 70 minutes. At the same time, a high-speed disperser was used at a speed of 3500 r / min to disperse the pigment evenly in the resin solution to obtain a pigment dispersion.

[0058] S3 Additive Mixing:

[0059] To the pigment dispersion, 4 g of plasticizer, DF677 silicone defoamer, 0.6g BYK-358N acrylate leveling agent, 0.5g cold resistance synergist, 0.6g glycerol antifreeze, stir at a stirring speed of 250r / min for 45 minutes to fully mix the additives;

[0060] S4 grinding and refining:

[0061] The mixed ink is ground through a three-roll mill for three times, and the fineness of the ink is controlled at 14 μm to improve the uniformity of the ink and the printing quality;

[0062] S5 filter packaging:

[0063] The ground ink is filtered using a filter membrane with a pore size of 8 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0064] The cold-resistant solvent is ethylene glycol ethyl ether.

[0065] The pigment is carbon black.

[0066] The plasticizer is dioctyl sebacate.

[0067] The preparation method of the cold-resistant synergist is:

[0068] T1: 18 g of 2-ethynylquinoline and 2 g of ethynylphenyl sulfide were added to 240 g of N,N-dimethylformamide, followed by the addition of 29 g of diphenylphosphoryl azide, 0.3 g of cuprous bromide, and 0.5 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture was stirred at 55°C and 220 rpm for 5 hours. The reaction progress was monitored by high performance liquid chromatography. The reaction was considered complete when the content of the azide compound no longer changed.

[0069] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 75°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0070] Example 3

[0071] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0072] S1 premix:

[0073] Add 30g of Baowei waterborne polyurethane resin 006 to 45g of cold-resistant solvent and stir at room temperature at a stirring speed of 200r / min for 50 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0074] S2 pigment dispersion:

[0075] 18 g of pigment and 1.3 g of fatty acid polyethylene glycol ester PEG400DL dispersant were added to the resin solution, the stirring speed was increased to 450 r / min, and the mixture was stirred for 80 minutes. At the same time, a high-speed disperser was used at a speed of 4500 r / min to disperse the pigment evenly in the resin solution to obtain a pigment dispersion.

[0076] S3 Additive Mixing:

[0077] To the pigment dispersion, 7g of plasticizer, DF677 silicone defoamer, 0.8g BYK-358N acrylate leveling agent, 0.8g cold resistance synergist, and 0.8g glycerol antifreeze were stirred at a stirring speed of 250r / min for 55 minutes to ensure that all additives were fully mixed.

[0078] S4 grinding and refining:

[0079] The mixed ink is ground through a three-roll mill for three times, and the fineness of the ink is controlled at 12 μm to improve the uniformity of the ink and the printing quality;

[0080] S5 filter packaging:

[0081] The ground ink is filtered using a filter membrane with a pore size of 6 μm to remove impurities and large particles, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0082] The cold-resistant solvent is propylene glycol methyl ether.

[0083] The pigment is phthalocyanine blue.

[0084] The plasticizer is diisononyl adipate.

[0085] The preparation method of the cold-resistant synergist is:

[0086] T1: Add 23 g of 2-ethynylquinoline and 2 g of ethynylphenyl sulfide to 280 g of N,N-dimethylformamide, and then add 32 g of diphenylphosphoryl azide, 0.5 g of cuprous bromide, and 0.7 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture is stirred at 65°C and 240 rpm for 5 hours. The reaction progress is monitored by high performance liquid chromatography. The reaction is considered complete when the content of the azide compound no longer changes.

[0087] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 75°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0088] Example 4

[0089] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0090] S1 premix:

[0091] Add 35g of Baowei waterborne polyurethane resin 006 to 50g of cold-resistant solvent and stir at room temperature at a stirring speed of 250r / min for 60 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0092] S2 pigment dispersion:

[0093] Add 20 g of pigment and 1.5 g of fatty acid polyethylene glycol ester PEG400DL dispersant to the resin solution, increase the stirring speed to 500 r / min, and stir for 90 minutes; at the same time, use a high-speed disperser at a speed of 5000 r / min to disperse the pigment at 5000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0094] S3 Additive Mixing:

[0095] To the pigment dispersion, 8g of plasticizer, DF677 silicone defoamer, 1g BYK-358N acrylate leveling agent, 1g cold resistance synergist, and 1g glycerol antifreeze were stirred at a stirring speed of 300 r / min for 60 minutes to ensure that all additives were fully mixed.

[0096] S4 grinding and refining:

[0097] The mixed ink is ground through a three-roll mill for 4 times, and the fineness of the ink is controlled at 10 μm to improve the uniformity of the ink and the printing quality;

[0098] S5 filter packaging:

[0099] The ground ink is filtered using a filter membrane with a pore size of 5 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0100] The cold-resistant solvent is propylene glycol methyl ether.

[0101] The pigment is quinacridone red.

[0102] The plasticizer is diisononyl adipate.

[0103] The preparation method of the cold-resistant synergist is:

[0104] T1: 26 g of 2-ethynylquinoline and 3 g of ethynylphenyl sulfide were added to 300 g of N,N-dimethylformamide, followed by the addition of 34 g of diphenylphosphoryl azide, 0.6 g of cuprous bromide, and 0.8 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture was stirred at 70°C and 250 rpm for 6 hours. The reaction progress was monitored by high performance liquid chromatography. The reaction was considered complete when the content of the azide compound no longer changed.

[0105] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 80°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0106] Comparative Example 1

[0107] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0108] S1 premix:

[0109] Add 20g of Baowei waterborne polyurethane resin 006 to 30g of cold-resistant solvent and stir at room temperature at a stirring speed of 150r / min for 30 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0110] S2 pigment dispersion:

[0111] Add 10 g of pigment and 0.5 g of fatty acid polyethylene glycol ester PEG400DL dispersant to the resin solution, increase the stirring speed to 300 / min, and stir for 60 minutes; at the same time, use a high-speed disperser at a speed of 3000 r / min to disperse the pigment at a speed of 3000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0112] S3 Additive Mixing:

[0113] To the pigment dispersion, 3 g of plasticizer, DF677 silicone defoamer, 0.5g BYK-358N acrylate leveling agent, and 0.5g glycerol antifreeze were stirred at a stirring speed of 200 r / min for 40 minutes to ensure that all additives were fully mixed.

[0114] S4 grinding and refining:

[0115] The mixed ink is ground through a three-roll mill for 2 times, and the fineness of the ink is controlled at 15μm to improve the uniformity of the ink and the printing quality;

[0116] S5 filter packaging:

[0117] The ground ink is filtered using a filter membrane with a pore size of 10 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0118] The cold-resistant solvent is ethylene glycol ethyl ether.

[0119] The pigment is titanium dioxide.

[0120] The plasticizer is dioctyl sebacate.

[0121] Comparative Example 2

[0122] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0123] S1 premix:

[0124] Add 20g of Baowei waterborne polyurethane resin 006 to 30g of cold-resistant solvent and stir at room temperature at a stirring speed of 150r / min for 30 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0125] S2 pigment dispersion:

[0126] Add 10 g of pigment and 0.5 g of fatty acid polyethylene glycol ester PEG400DL dispersant to the resin solution, increase the stirring speed to 300 / min, and stir for 60 minutes; at the same time, use a high-speed disperser at a speed of 3000 r / min to disperse the pigment at a speed of 3000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0127] S3 Additive Mixing:

[0128] To the pigment dispersion, 3 g of plasticizer, DF677 silicone defoamer, 0.5g BYK-358N acrylate leveling agent, 0.1g cold resistance synergist, 0.5g glycerol antifreeze, stir at a stirring speed of 200r / min for 40 minutes to fully mix the additives;

[0129] S4 grinding and refining:

[0130] The mixed ink is ground through a three-roll mill for 2 times, and the fineness of the ink is controlled at 15μm to improve the uniformity of the ink and the printing quality;

[0131] S5 filter packaging:

[0132] The ground ink is filtered using a filter membrane with a pore size of 10 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0133] The cold-resistant solvent is ethylene glycol ethyl ether.

[0134] The pigment is titanium dioxide.

[0135] The plasticizer is dioctyl sebacate.

[0136] The preparation method of the cold-resistant synergist is:

[0137] T1: 13 g of 2-ethynylquinoline was added to 200 g of N,N-dimethylformamide, followed by the addition of 27 g of diphenylphosphoryl azide, 0.2 g of cuprous bromide, and 0.4 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture was stirred at 200 rpm at 50°C for 4 hours. The reaction progress was monitored by high performance liquid chromatography. The reaction was considered complete when the content of the azide compound no longer changed.

[0138] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 70°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0139] Comparative Example 3

[0140] A method for preparing cold-resistant low-temperature ink, the operating steps of which are as follows:

[0141] S1 premix:

[0142] Add 20g of Baowei waterborne polyurethane resin 006 to 30g of cold-resistant solvent and stir at room temperature at a stirring speed of 150r / min for 30 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution;

[0143] S2 pigment dispersion:

[0144] Add 10 g of pigment and 0.5 g of fatty acid polyethylene glycol ester PEG400DL dispersant to the resin solution, increase the stirring speed to 300 / min, and stir for 60 minutes; at the same time, use a high-speed disperser at a speed of 3000 r / min to disperse the pigment at a speed of 3000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion;

[0145] S3 Additive Mixing:

[0146] To the pigment dispersion, 3 g of plasticizer, DF677 silicone defoamer, 0.5g BYK-358N acrylate leveling agent, 0.1g cold resistance synergist, 0.5g glycerol antifreeze, stir at a stirring speed of 200r / min for 40 minutes to fully mix the additives;

[0147] S4 grinding and refining:

[0148] The mixed ink is ground through a three-roll mill for 2 times, and the fineness of the ink is controlled at 15μm to improve the uniformity of the ink and the printing quality;

[0149] S5 filter packaging:

[0150] The ground ink is filtered using a filter membrane with a pore size of 10 μm to remove impurities and large particles therein, and the filtered ink is then placed in a packaging container to obtain cold-resistant and low-temperature ink.

[0151] The cold-resistant solvent is ethylene glycol ethyl ether.

[0152] The pigment is titanium dioxide.

[0153] The plasticizer is dioctyl sebacate.

[0154] The preparation method of the cold-resistant synergist is:

[0155] T1: 13 g of 2-ethynylquinoline and 1 g of ethynylphenyl sulfide were added to 200 g of N,N-dimethylformamide, followed by the addition of 0.2 g of cuprous bromide and 0.4 g of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture was stirred at 200 rpm at 50°C for 4 hours. The reaction progress was monitored by high performance liquid chromatography. The reaction was considered complete when the content of the azide compound no longer changed.

[0156] T2: After the reaction is completed, the mixture is filtered and the filtrate is transferred to a vacuum distillation apparatus and subjected to vacuum distillation at 70°C to remove excess N,N-dimethylformamide to obtain a cold-resistant synergist.

[0157] Ink flow time / second Ink drying time / minute Adhesion Example 1 39 28 No obvious shedding phenomenon Example 2 37 27 No obvious shedding phenomenon Example 3 35 25 No obvious shedding phenomenon Example 4 33 24 No obvious shedding phenomenon Comparative Example 1 90 65 A lot of ink is falling off Comparative Example 2 48 36 A small amount of ink is falling off Comparative Example 3 45 33 A small amount of ink is falling off

[0158] Through the data analysis of the above examples and comparative examples, the ink prepared by the present invention has good fluidity at low temperatures, fast drying speed and strong adhesion.

[0159] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as above in terms of a preferred embodiment, it is not intended to limit the present invention. Any person skilled in the art can, without departing from the scope of the technical solution of the present invention, make some changes or modifications to equivalent embodiments using the technical contents disclosed above. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a cold-resistant low-temperature ink, the operating steps of which are: S1 premix: Add 20-35 parts of polyurethane resin to 30-50 parts of cold-resistant solvent, and stir at room temperature at a stirring speed of 150-250 r / min for 30-60 minutes to fully dissolve the polyurethane resin in the cold-resistant solvent to form a uniform resin solution; S2 pigment dispersion: Add 10-20 parts of pigment and 0.5-1.5 parts of fatty acid polyethylene glycol ester dispersant to the resin solution, increase the stirring speed to 300-500 r / min, and stir for 60-90 minutes; at the same time, use a high-speed disperser at a speed of 3000-5000 r / min to disperse the pigment at a speed of 3000-5000 r / min to ensure that the pigment is evenly dispersed in the resin solution to obtain a pigment dispersion; S3 Additive Mixing: Add 3-8 parts of plasticizer, 0.5-1 part of silicone defoamer, 0.5-1 part of acrylate leveling agent, 0.1-1 part of cold resistance synergist, and 0.5-1 part of glycerol antifreeze to the pigment dispersion in sequence, and stir at a stirring speed of 200-300 r / min for 40-60 minutes to fully mix the additives; S4 grinding and refining: Grind the mixed ink through a three-roll mill for 2-4 times, controlling the fineness of the ink to be between 10-15 μm to improve the uniformity of the ink and the printing quality; S5 filter packaging: The ground ink is filtered using a filter membrane with a pore size of 5-10 μm to remove impurities and large particles, and then the filtered ink is placed in a packaging container to obtain cold-resistant and low-temperature ink; The cold-resistant synergist is prepared by reacting 2-ethynylquinoline, ethynylphenyl sulfide, diphenylphosphoryl azide, cuprous bromide and N,N,N',N",N"-pentamethyldiethylenetriamine.

2. The method for preparing a cold-resistant and low-temperature ink according to claim 1, characterized in that: The cold-resistant solvent is ethylene glycol ethyl ether or propylene glycol methyl ether.

3. The method for preparing a cold-resistant and low-temperature ink according to claim 1, wherein: The pigment is one of titanium dioxide, carbon black, phthalocyanine blue and quinacridone red.

4. The method for preparing a cold-resistant and low-temperature ink according to claim 1, wherein: The plasticizer is dioctyl sebacate or diisononyl adipate.

5. The method for preparing a cold-resistant and low-temperature ink according to claim 1, characterized in that: The preparation method of the cold-resistant synergist is: T1: Add 13-26 parts of 2-ethynylquinoline and 1-3 parts of ethynylphenyl sulfide to 200-300 parts of N,N-dimethylformamide, and then add 27-34 parts of diphenylphosphoryl azide, 0.2-0.6 parts of cuprous bromide, and 0.4-0.8 parts of N,N,N',N",N"-pentamethyldiethylenetriamine. The mixture is stirred at 50-70°C and 200-250 rpm for 4-6 hours. The reaction progress is monitored by high performance liquid chromatography. The reaction is considered complete when the content of the azide compound no longer changes. T2: After the reaction is completed, filter and then transfer the filtrate to a vacuum distillation apparatus, and perform vacuum distillation at a temperature of 70-80°C to remove excess N,N-dimethylformamide to obtain a cold resistance enhancer.