Preparation method of special halogen-free ink for coating black film on lithium battery

Abstract

The invention relates to a preparation method of halogen-free ink special for a lithium battery coating black film, and belongs to the technical field of ink. The preparation method comprises the following steps: heating, stirring and uniformly mixing distilled water, pigment, a thickening agent, a sweetening agent and a novel non-toxic antioxidant; continuously adding a connecting material, completely emulsifying, and standing to obtain the halogen-free ink special for the lithium battery coating black film; the novel non-toxic antioxidant disclosed by the invention is prepared from sulfydryl-beta-cyclodextrin, potassium sorbate, sodium bicarbonate and vitamin C; the special halogen-free ink prepared by the invention is not easy to fade and has good printing performance.

Description

Technical Field

[0001] This invention relates to the field of ink technology, and in particular to a method for preparing a halogen-free ink specifically for lithium battery coating black film. Background Technology

[0002] With my country's increasing emphasis on green, environmentally friendly, and sustainable social development, and the growing public awareness of environmental protection, edible inks, as a new type of green and environmentally friendly ink, have become a hot topic of social attention in recent years. Because of their inherent safety (being safe for consumption), edible inks can be printed on food and pharmaceutical packaging, making them a highly sought-after printing ink with wide applications across various fields.

[0003] Chinese Patent CN103224730B relates to a method for preparing a halogen-free ink specifically for lithium battery coating black film, which aims to solve the problem of poor high-temperature resistance of existing edible inks. The heat-resistant edible ink is made from distilled water, potassium sorbate, sucrose, xanthan gum, soybean oil, food coloring, and a heat-resistant reagent by weight percentage. Preparation method: 1. Weigh each raw material according to the weight percentage; 2. Dissolve potassium sorbate in distilled water to obtain a potassium sorbate solution; 3. Add sucrose to the potassium sorbate solution, then add xanthan gum; 4. Mix soybean oil, food coloring, and the heat-resistant reagent; 5. Add the solution obtained in step 4 to the solution obtained in step 3, stir, and let stand to obtain the heat-resistant edible ink.

[0004] Chinese Patent CN105331194B discloses a nanocrystalline cellulose edible ink and its preparation method. The method involves mixing nanocrystalline cellulose with water, ultrasonically treating the mixture, and then adding water, sweetener, colorant, thickener, and binder in batches under constant temperature and stirring conditions to obtain the nanocrystalline cellulose edible ink. The nanocrystalline cellulose used in this method is derived from natural plant fibers.

[0005] Chinese Patent CN109971248A: This invention relates to a method for preparing a halogen-free ink specifically for lithium battery coating black film, belonging to the field of printing materials technology. The invention uses squid ink or carrot pigment as a colorant, soybean oil as a binder, gelatin-modified chitosan as a thickener, soybean lecithin as an emulsifier, and sucrose aqueous solution as a sweetener to prepare an edible ink.

[0006] The inks prepared using the above patents and existing technologies are prone to fading and have unsatisfactory printing performance. Summary of the Invention

[0007] To address the above problems, this invention provides a method for preparing a halogen-free ink specifically for lithium battery coating black films, the steps of which are as follows: S1: According to the weight parts, add 80-100 parts distilled water, 1-5 parts colorant, 0.2-2 parts thickener, 0.1-1 part sweetener, and 0.02-0.06 parts of novel non-toxic antioxidant, heat to 40-50℃, and stir to mix evenly; S2: Continue to add 5-15 parts of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film.

[0008] As a supplement to the present invention, the colorant is one of the following: sodium copper chlorophyllin, natural plant carbon black, carmine, grape skin red, paprika red, turmeric, squid ink, and carotene.

[0009] As a supplement to the present invention, the thickener is one of gum arabic, pectin, carrageenan, xanthan gum, and starch.

[0010] As a supplement to the present invention, the sweetener is one of glucose, sorbitol, and sucrose.

[0011] As a supplement to the present invention, the binder is one of peanut oil, salad oil, and soybean oil.

[0012] As a supplement to the present invention, the settling time of S2 is 30-60 minutes.

[0013] As a supplement to the present invention, the preparation method of the novel non-toxic antioxidant is as follows: A1: Add 11-22 parts of mercapto-β-cyclodextrin (CAS No. 81644-55-5), 5-10 parts of potassium sorbate, 1-3 parts of sodium bicarbonate, and 0.05-0.3 parts of vitamin C to a reaction vessel, and add 200-240 parts of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 50-60℃ and stir continuously for 3-5 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 100-200 parts of ethanol, and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

[0014] Reaction mechanism The thiol group (-SH) in mercapto-β-cyclodextrin exhibits relatively low electronegativity of the sulfur atom, while its hydrogen atom possesses a certain degree of reactivity. Under heating and stirring conditions, the hydrogen atom on the thiol group readily dissociates, forming a thiol anion (-S-).

[0015] The carbon-carbon double bond formed by vitamin C is electrophilic. The thiol anion acts as a nucleophile, attacking the carbon-carbon double bond and undergoing a Michael addition reaction to form a new carbon-sulfur bond.

[0016] The active groups such as carbon-carbon double bonds in potassium sorbate molecules undergo Michael addition reactions with mercapto-β-cyclodextrin to form new carbon-sulfur bonds, generating a novel non-toxic antioxidant with antioxidant properties.

[0017] Technical effect The present invention discloses a method for preparing a halogen-free ink for lithium battery coating black film. Compared with the prior art, the present invention has the following significant advantages: 1. Highly effective antioxidant: The novel non-toxic antioxidant prepared by this invention contains a variety of active groups, which can effectively capture free radicals generated during ink oxidation, interrupt the oxidation chain reaction, prevent the binder and other components in the ink from oxidizing and deteriorating, and significantly extend the shelf life of the ink.

[0018] 2. Maintains color and performance stability: By inhibiting oxidation, this antioxidant maintains the original color of the ink, ensuring the vibrancy and clarity of the printed pattern. Simultaneously, it ensures the stability of key performance indicators such as the ink's rheological properties and drying properties, thus improving printing quality. Detailed Implementation

[0019] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the following detailed description is provided in conjunction with embodiments and comparative examples: 1. Color intensity determination: The test shall be conducted in accordance with GB / T15962-1995; 2. Flowability determination: The test shall be conducted in accordance with GB / T14624.3-93 "Test Method for Flowability of Ink"; 3. Ink tinting strength test: The test shall be conducted in accordance with GB / T14624.2-93 "Ink Tinting Strength Test Method".

[0020] Example 1 A method for preparing a halogen-free ink specifically for coating black films in lithium batteries, comprising the following steps: S1: Heat 80g distilled water, 1g colorant, 0.2g thickener, 0.1g sweetener, and 0.02g novel non-toxic antioxidant to 40℃ and stir until well mixed; S2: Continue to add 5g of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film.

[0021] The colorant mentioned is sodium copper chlorophyllin.

[0022] The thickener is gum arabic.

[0023] The sweetener is glucose.

[0024] The binder is peanut oil.

[0025] The settling time for S2 is 30 minutes.

[0026] The preparation method of the novel non-toxic antioxidant is as follows: A1: Add 11g of mercapto-β-cyclodextrin (CAS No. 81644-55-5), 5g of potassium sorbate, 1g of sodium bicarbonate, and 0.05g of vitamin C to a reaction vessel, and add 200g of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 50℃ and stir continuously for 3 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 100g of ethanol and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

[0027] Example 2 A method for preparing a halogen-free ink specifically for coating black films in lithium batteries, comprising the following steps: S1: Heat 85g distilled water, 2g colorant, 1g thickener, 0.5g sweetener, and 0.03g novel non-toxic antioxidant to 45℃ and stir until well mixed. S2: Continue to add 8g of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film.

[0028] The pigment mentioned is natural plant-based carbon black.

[0029] The thickener is pectin.

[0030] The sweetener mentioned is sorbitol.

[0031] The binder is salad oil.

[0032] The settling time for S2 is 40 minutes.

[0033] The preparation method of the novel non-toxic antioxidant is as follows: A1: Add 15g of mercapto-β-cyclodextrin (CAS No. 81644-55-5), 6g of potassium sorbate, 2g of sodium bicarbonate, and 0.1g of vitamin C to a reaction vessel, and add 210g of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 55°C and stir continuously for 4 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 140g of ethanol and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

[0034] Example 3 A method for preparing a halogen-free ink specifically for coating black films in lithium batteries, comprising the following steps: S1: Heat 95g distilled water, 4g colorant, 1.5g thickener, 0.8g sweetener, and 0.05g novel non-toxic antioxidant to 45℃ and stir until well mixed. S2: Continue to add 13g of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film.

[0035] The pigment mentioned is carmine.

[0036] The thickener is carrageenan.

[0037] The sweetener mentioned is sorbitol.

[0038] The binder is salad oil.

[0039] The settling time for S2 is 50 minutes.

[0040] The preparation method of the novel non-toxic antioxidant is as follows: A1: Add 20g of mercapto-β-cyclodextrin (CAS No. 81644-55-5), 8g of potassium sorbate, 2g of sodium bicarbonate, and 0.2g of vitamin C to a reaction vessel, and add 230g of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 55℃ and stir continuously for 4 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 180g of ethanol and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

[0041] Example 4 A method for preparing a halogen-free ink specifically for coating black films in lithium batteries, comprising the following steps: S1: Heat 100g distilled water, 5g colorant, 2g thickener, 1g sweetener, and 0.06g novel non-toxic antioxidant to 50℃ and stir until well mixed. S2: Continue to add 15g of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film.

[0042] The colorant mentioned is carotene.

[0043] The thickener is starch.

[0044] The sweetener is sucrose.

[0045] The binder is soybean oil.

[0046] The settling time for S2 is 60 minutes.

[0047] The preparation method of the novel non-toxic antioxidant is as follows: A1: Add 22g of mercapto-β-cyclodextrin (CAS No. 81644-55-5), 10g of potassium sorbate, 3g of sodium bicarbonate, and 0.3g of vitamin C to a reaction vessel, and add 240g of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 60℃ and stir continuously for 5 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 200g of ethanol and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

[0048] Comparative Example 1 No novel non-toxic antioxidants were added; otherwise, it was the same as in Example 1.

[0049] Comparative Example 2 Without adding potassium sorbate, everything else is the same as in Example 1.

[0050] Comparative Example 3 Vitamin C was not added; otherwise, it was the same as in Example 1.

[0051] The test results of the examples and comparative examples are shown in Table 1.

[0052] Table 1: Test Results of Examples and Comparative Examples Based on the data analysis of the above embodiments and comparative examples, the halogen-free ink for lithium battery coating black film prepared by the present invention is not easy to fade and has good printing performance.

[0053] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a halogen-free ink specifically for coating black films in lithium batteries, comprising the following steps: S1: According to the weight parts, add 80-100 parts distilled water, 1-5 parts colorant, 0.2-2 parts thickener, 0.1-1 part sweetener, and 0.02-0.06 parts of novel non-toxic antioxidant, heat to 40-50℃, and stir to mix evenly; S2: Continue to add 5-15 parts of binder material, emulsify completely, and let stand to obtain halogen-free ink for lithium battery coating black film. The novel non-toxic antioxidant is prepared by reacting mercapto-β-cyclodextrin, potassium sorbate, sodium bicarbonate, and vitamins.

2. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The colorant mentioned is one of the following: sodium copper chlorophyllin, natural plant carbon black, carmine, grape skin red, paprika red, turmeric, squid ink, and carotene.

3. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The thickener is one of gum arabic, pectin, carrageenan, xanthan gum, and starch.

4. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The sweetener is one of glucose, sorbitol, and sucrose.

5. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The binder is one of peanut oil, salad oil, or soybean oil.

6. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The settling time for S2 is 30-60 minutes.

7. The method for preparing a halogen-free ink for lithium battery coating black film according to claim 1, characterized in that: The preparation method of the novel non-toxic antioxidant is as follows: A1: Add 11-22 parts of mercapto-β-cyclodextrin, 5-10 parts of potassium sorbate, 1-3 parts of sodium bicarbonate, and 0.05-0.3 parts of vitamin C to a reaction vessel, and add 200-240 parts of deionized water as a solvent to fully dissolve the raw materials; under nitrogen protection, heat the reaction system to 50-60℃ and stir continuously for 3-5 hours. A2: After the reaction is complete, the reaction solution is cooled to room temperature, and then water is removed by rotary evaporator. Next, the remaining liquid is freeze-dried to obtain crude product. The crude product is dissolved in 100-200 parts of ethanol, and then purified by silica gel column chromatography. The eluent containing the target product is collected and freeze-dried again to finally obtain a pure new non-toxic antioxidant.

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