Environment-friendly plant-based odorless quick-dry ink and preparation method thereof
Environmentally friendly plant-based inks, modified by transesterification and vacuum distillation, solve the problems of long surface drying time and odor, achieving adaptability and environmental friendliness for high-speed printing, and are suitable for food packaging, children's books and other applications.
Patent Information
- Application Number
- CN202511059127.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-30
- Publication Date
- 2025-10-31
AI Technical Summary
Existing plant-based inks have long surface drying times, making them difficult to adapt to the production pace of high-speed printing. They also contain free fatty acids and aldehydes, which cause odors and affect the use of printed products.
The vegetable oil is treated with transesterification. Through the synergistic effect of transesterification modified binder and castor oil-based acrylate, the ink film-forming process is accelerated. Vacuum distillation is used to remove odor components, and the low-toxicity antioxidant di-tert-butyl-p-cresol is used to inhibit oxidation. Carboxylated cellulose nanocrystals are added to improve dispersibility.
It significantly shortens surface drying time to within 2 hours, reduces odor, improves printing efficiency, and is suitable for odor-sensitive applications such as food packaging and children's books. It is also more environmentally friendly, has good storage stability, and aligns with the trend of green development.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of ink technology, specifically to an environmentally friendly plant-based, odor-free, quick-drying ink and its preparation method. Background Technology
[0002] As a core material in packaging printing, publication printing, and commercial printing, printing inks have seen their market size continue to expand with the development of the global printing industry. Traditional inks mainly use mineral oils such as gasoline and kerosene derivatives as raw materials. However, with increasingly stringent environmental protection requirements for printing inks, plant-based inks have effectively reduced VOC emissions compared to traditional inks, making them the main environmentally friendly ink products.
[0003] However, in existing technologies, existing plant-based inks such as soybean ink have a high content of unsaturated fatty acids and a slow oxidation polymerization rate, resulting in a long surface drying time for the ink, making it difficult to adapt to the production rhythm of high-speed printing. In addition, plant oils contain free fatty acids and aldehydes, which can produce natural oil odors, especially in sealed packaging environments, which are more noticeable and affect the use of printed products. Summary of the Invention
[0004] The purpose of this invention is to provide an environmentally friendly, plant-based, odor-free, and quick-drying ink and its preparation method, in order to solve the problems mentioned in the background art, such as the long surface drying time of existing plant-based inks, which are difficult to adapt to the production rhythm of high-speed printing, and the fact that plant oils contain free fatty acids and aldehydes, which will produce natural oil odors.
[0005] To achieve the above objectives, the present invention provides the following technical solution: an environmentally friendly plant-based, odor-free, quick-drying ink, comprising the following raw materials in parts by weight: 20-28 parts pigment powder, 55-65 parts binder, 1.5-3 parts dispersant, 0.1-0.3 parts drier, 0.1-0.25 parts defoamer, 1-2 parts castor oil-based acrylate, and 1-5 parts di-tert-butyl-p-cresol; the binder is made from the following raw materials: 45-50 parts linseed oil, 15-20 parts castor oil, 25-30 parts soybean oil, 20-30 parts methanol, and 0.5-1 part potassium hydroxide; linseed oil... The material primarily uses oil, castor oil, and soybean oil, completely eliminating petroleum-based raw materials. Modification through transesterification of methanol and potassium hydroxide optimizes the molecular structure of the vegetable oils, improving drying speed and making their viscosity more suitable for transfer requirements in the printing process. Simultaneously, the drying characteristics, i.e., the rate of oxidative polymerization, are significantly enhanced, while retaining the environmental and odor-neutralizing advantages of plant-based materials. Carboxylated cellulose nanocrystals and castor oil-based acrylates are both plant-derived, exhibiting good compatibility with the system and avoiding the risk of contamination from synthetic chemical auxiliaries. Di-tert-butyl-p-cresol is a low-toxicity antioxidant that inhibits oxidative rancidity of vegetable oils, meeting the safety requirements for food contact materials.
[0006] Preferably, the pigment powder is selected from any one of phthalocyanine blue, phthalocyanine red, and iron oxide yellow.
[0007] Preferably, the dispersant is carboxylated cellulose nanocrystals.
[0008] Preferably, the drying agent is selected from either cobalt isooctanoate or manganese isooctanoate.
[0009] A method for preparing an environmentally friendly, plant-based, odor-free, quick-drying ink includes the following steps: I. Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil, and vacuum dehydrate and vacuum distill to remove low-boiling-point odor components, then mix them for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately, and vacuum calcine the pigment powder and cool it for later use. II. Preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at a speed of 200-300 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 60-65℃ and react at a constant temperature for 2-3 hours. Take samples every 30 minutes to test the acid value. When the acid value stabilizes below 5 mg KOH / g, stop the reaction. Post-process the product to obtain the transesterification modified binder. III. Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.08 to -0.1 MPa, and slowly add the treated pigment powder and dispersant while stirring at a speed of 500-800 r / min. Stir for 30 to 60 minutes to initially disperse the pigment. Then, send it to a three-roll mill, control the grinding temperature at 40 to 50°C, and simultaneously purge nitrogen to grind until the ink fineness reaches 10 to 15 μm. IV. Ink Preparation: Place the ground material into a mixing container, vacuum to -0.08 to -0.1 MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, and stir at 300-500 r / min for 20-40 minutes to ensure uniform dispersion of the additives before discharging to obtain ink. V. The finished ink is degassed by a vacuum degassing machine to remove microbubbles and impurities are removed by a precision filter to obtain the finished ink. The ink is then filled into aluminum cans under nitrogen cover and stored in a sealed, light-proof container.
[0010] Preferably, in step I, the flaxseed oil, soybean oil and castor oil are mixed in a ratio of 5:3:2 and stirred for 30 minutes under vacuum of -0.09 MPa and temperature of 60°C to dehydrate the mixture, so that the moisture content is controlled below 0.1%.
[0011] Preferably, in step I, the pigment powder is calcined at a temperature of 500-800°C for 2-4 hours to remove adsorbed organic impurities and volatile odor substances from the surface.
[0012] Preferably, in step II, the post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40℃, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 6-7, allow to stand and separate into layers, then remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 6.9-7.1. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder.
[0013] Compared with the prior art, the beneficial effects of the present invention are: 1. In this invention, the ink film-forming process is accelerated by the synergistic effect of transesterified binder and castor oil-based acrylate. Transesterification optimizes the molecular structure of vegetable oil and improves the oxidative crosslinking rate. Castor oil-based acrylate introduces double bonds, promotes photo / thermal polymerization reaction, significantly shortens the surface drying time, and reduces the actual drying time to within 2 hours, greatly reducing the waiting time after printing, adapting to high-speed production lines, and improving printing and processing efficiency. 2. In this invention, by performing a vacuum distillation deodorization process on the binder, low-boiling-point odor components such as free fatty acids and aldehydes in vegetable oil are precisely removed. Combined with the synergistic effect of the low-odor drying agent cobalt isooctanoate and antioxidants, the odor of the ink is greatly reduced, solving the problem of strong odor in traditional plant-based inks. It can be directly applied to food packaging, children's books, baby products and other odor-sensitive scenarios, improving the safety of end products. 3. This invention uses plant-based raw materials as the core and modifies the plant oil binder through transesterification reaction, reducing the dependence of traditional inks on mineral oil and synthetic resins. This makes the invention more environmentally friendly and in line with the trend of green development. In addition, the production process removes low-boiling-point impurities through vacuum distillation, with no additional pollutant emissions. 4. In this invention, the viscosity of the binder is stabilized by transesterification, and the dispersing effect of carboxylated cellulose nanocrystals ensures uniform transfer during printing without smearing or missing prints. At the same time, the addition of di-tert-butyl-p-cresol antioxidant results in low viscosity change rate during long-term storage, no sedimentation or stratification, extending the shelf life of this invention and reducing losses caused by storage deterioration. Detailed Implementation
[0014] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0015] The present invention will be further described below with reference to embodiments.
[0016] Example 1: This example provides an environmentally friendly plant-based, odorless, quick-drying ink, comprising the following raw materials in parts by weight: 22 parts pigment powder, 58 parts binder, 2 parts dispersant, 0.2 parts drier, 0.15 parts defoamer (selected from Evonik: TEGO® Foamex 16), 1.5 parts castor oil-based acrylate (selected from Jinan Hongxin Chemical Co., Ltd.), and 3 parts di-tert-butyl-p-cresol (BHT, selected from Lanxess: PUROLANBHT). The binder is made from the following raw materials: 48 parts flaxseed oil (commercially available), 18 parts castor oil (commercially available), 27 parts soybean oil (commercially available), 25 parts methanol (Sigma-Aldrich: Methanol), and 0.8 parts potassium hydroxide (Sigma-Aldrich: Potassium Hydroxide Pellets). The pigment powder is selected from any one of Phthalocyanine Blue (BASF Pigment Blue), Phthalocyanine Red (Clariant PV FastRed E3B), and Iron Oxide Yellow (Guotai Pigment YA23HR); the dispersant is selected from carboxylated cellulose nanocrystals (produced by Guilin Qihong Technology Co., Ltd.); and the drying agent is selected from cobalt isooctanoate.
[0017] This embodiment also provides a method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink, including the following steps: Step 1: Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil and stir them separately for 30 minutes under vacuum of -0.09MPa and temperature of 60℃ to dehydrate them, so that the moisture content is controlled below 0.1%. Vacuum distillation is used to remove low-boiling-point odor components. Then mix them in a ratio of 5:3:2 for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately. Vacuum calcination of pigment powder is carried out and then cooled for later use. The high-temperature calcination temperature is 600℃ and calcination is carried out for 2 hours to remove surface-adsorbed organic impurities and volatile odor substances. Step 2, preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at a speed of 200 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 60℃ and keep it at a constant temperature for 2 hours. Take samples every 30 minutes to test the acid value (free fatty acid content). When the acid value stabilizes below 5 mg KOH / g, stop the reaction and perform post-treatment on the product to obtain the transesterification modified binder. The post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40℃, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 6, allow to stand and separate into layers, and remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 6.9. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder. Step 3, Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.08MPa, and slowly add the treated pigment powder and dispersant while stirring at 500r / min. Stir for 30 minutes to initially disperse the pigment. Then, send it to a three-roll mill, control the grinding temperature at 40℃, and simultaneously pass nitrogen gas through the mill to make the ink fineness reach 10μm. Step 4, Ink Preparation: Place the ground material into a mixing container, vacuum to -0.08 to -0.1 MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, stir at 300-500 r / min for 20-40 minutes to ensure uniform dispersion of the additives, and then discharge the material to obtain ink. Step 5: Remove microbubbles from the prepared ink using a vacuum degassing machine and remove impurities using a precision filter to obtain the finished ink. Fill the ink into aluminum cans under nitrogen cover and store them in a sealed, light-proof container.
[0018] Example 2: This example provides an environmentally friendly plant-based, odorless, quick-drying ink, comprising the following raw materials in parts by weight: 25 parts pigment powder, 62 parts binder, 2.5 parts dispersant, 0.3 parts drier, 0.2 parts defoamer, 2 parts castor oil-based acrylate, and 5 parts di-tert-butyl-p-cresol; the binder is made from the following raw materials: 50 parts linseed oil, 20 parts castor oil, 30 parts soybean oil, 30 parts methanol, and 1 part potassium hydroxide; The pigment powder is selected from any one of phthalocyanine blue, phthalocyanine red, and iron oxide yellow; the dispersant is selected from carboxylated cellulose nanocrystals; and the drying agent is selected from cobalt isooctanoate.
[0019] This embodiment also provides a method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink, including the following steps: Step 1: Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil and stir them separately for 30 minutes under vacuum of -0.09MPa and temperature of 60℃ to dehydrate them, so that the moisture content is controlled below 0.1%. Vacuum distillation is used to remove low-boiling-point odor components. Then mix them in a ratio of 5:3:2 for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately. Vacuum calcination of pigment powder is carried out and then cooled for later use. The high-temperature calcination temperature is 700℃ and calcination is carried out for 3 hours to remove surface-adsorbed organic impurities and volatile odor substances. Step 2, preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at 300 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 65℃ and react at a constant temperature for 3 hours. Take samples every 30 minutes to test the acid value (free fatty acid content). When the acid value stabilizes below 5 mg KOH / g, stop the reaction and perform post-processing on the product to obtain the transesterification modified binder. The post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40°C, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 7, allow to stand and separate into layers, and remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 7. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder. Step 3, Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.1MPa, and slowly add the treated pigment powder and dispersant while stirring at a speed of 500-800r / min. Stir for 60 minutes to initially disperse the pigment. Then, send it to a three-roll mill, control the grinding temperature at 50℃, and simultaneously introduce nitrogen gas to grind until the ink fineness reaches 15μm. Step 4, Ink Preparation: Place the ground material into a mixing container, vacuum to -0.1MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, stir at 500r / min for 40 minutes to ensure uniform dispersion of the additives, and then discharge the material to obtain ink. Step 5: Remove microbubbles from the prepared ink using a vacuum degassing machine and remove impurities using a precision filter to obtain the finished ink. Fill the ink into aluminum cans under nitrogen cover and store them in a sealed, light-proof container.
[0020] Example 3: This example provides an environmentally friendly plant-based, odorless, quick-drying ink, comprising the following raw materials in parts by weight: 20 parts pigment powder, 55 parts binder, 1.5 parts dispersant, 0.1 parts drier, 0.1 parts defoamer, 1 part castor oil-based acrylate, and 1 part di-tert-butyl-p-cresol; the binder is made from the following raw materials: 45 parts linseed oil, 15 parts castor oil, 25 parts soybean oil, 20 parts methanol, and 0.5 parts potassium hydroxide; The pigment powder is selected from any one of phthalocyanine blue, phthalocyanine red, and iron oxide yellow; the dispersant is selected from carboxylated cellulose nanocrystals; and the drying agent is selected from cobalt isooctanoate.
[0021] This embodiment also provides a method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink, including the following steps: Step 1: Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil and stir them separately for 30 minutes under vacuum of -0.09MPa and temperature of 60℃ to dehydrate them, so that the moisture content is controlled below 0.1%. Vacuum distillation is used to remove low-boiling-point odor components. Then mix them in a ratio of 5:3:2 for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately. Vacuum calcination of pigment powder is carried out and then cooled for later use. The high-temperature calcination temperature is 500℃ and calcination is carried out for 4 hours to remove surface-adsorbed organic impurities and volatile odor substances. Step 2, preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at 300 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 65℃ and react at a constant temperature for 3 hours. Take samples every 30 minutes to test the acid value (free fatty acid content). When the acid value stabilizes below 5 mg KOH / g, stop the reaction and perform post-processing on the product to obtain the transesterification modified binder. The post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40°C, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 7, allow to stand and separate into layers, and remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 7.1. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder. Step 3, Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.1MPa, and slowly add the treated pigment powder and dispersant while stirring at 800r / min. Stir for 60 minutes to initially disperse the pigment. Then send it to a three-roll mill, control the grinding temperature at 50℃, and simultaneously pass nitrogen gas through the mill to make the ink fineness reach 10μm. Step 4, Ink Preparation: Place the ground material into a mixing container, vacuum to -0.1MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, stir at 500r / min for 40 minutes to ensure uniform dispersion of the additives, and then discharge the material to obtain ink. Step 5: Remove microbubbles from the prepared ink using a vacuum degassing machine and remove impurities using a precision filter to obtain the finished ink. Fill the ink into aluminum cans under nitrogen cover and store them in a sealed, light-proof container.
[0022] Example 4: This example provides an environmentally friendly plant-based, odorless, quick-drying ink, comprising the following raw materials in parts by weight: 28 parts pigment powder, 65 parts binder, 3 parts dispersant, 0.3 parts drier, 0.25 parts defoamer, 1.8 parts castor oil-based acrylate, and 5 parts di-tert-butyl-p-cresol; the binder is made from the following raw materials: 47 parts linseed oil, 17 parts castor oil, 28 parts soybean oil, 28 parts methanol, and 0.7 parts potassium hydroxide; The pigment powder is selected from any one of phthalocyanine blue, phthalocyanine red, and iron oxide yellow; the dispersant is selected from carboxylated cellulose nanocrystals; and the drying agent is selected from cobalt isooctanoate.
[0023] This embodiment also provides a method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink, including the following steps: Step 1: Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil and stir them separately for 30 minutes under vacuum of -0.09MPa and temperature of 60℃ to dehydrate them, so that the moisture content is controlled below 0.1%. Vacuum distillation is used to remove low-boiling-point odor components. Then mix them in a ratio of 5:3:2 for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately. Vacuum calcination of pigment powder is carried out and then cooled for later use. The high-temperature calcination temperature is 800℃ and calcination is carried out for 3 hours to remove surface-adsorbed organic impurities and volatile odor substances. Step 2, preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at a speed of 200 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 60℃ and keep it at a constant temperature for 2 hours. Take samples every 30 minutes to test the acid value (free fatty acid content). When the acid value stabilizes below 5 mg KOH / g, stop the reaction and perform post-treatment on the product to obtain the transesterification modified binder. The post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40°C, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 7, allow to stand and separate into layers, and remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 7. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder. Step 3, Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.08MPa, and slowly add the treated pigment powder and dispersant while stirring at 500r / min. Stir for 30 minutes to initially disperse the pigment. Then, send it to a three-roll mill, control the grinding temperature at 40℃, and simultaneously pass nitrogen gas through the mill to make the ink fineness reach 10-15μm. Step 4, Ink Preparation: Place the ground material into a mixing container, vacuum to -0.08MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, stir at 400r / min for 20 minutes to ensure uniform dispersion of the additives, and then discharge the material to obtain ink. Step 5: Remove microbubbles from the prepared ink using a vacuum degassing machine and remove impurities using a precision filter to obtain the finished ink. Fill the ink into aluminum cans under nitrogen cover and store them in a sealed, light-proof container.
[0024] Comparative Example 1: The environmentally friendly plant-based odor-free quick-drying ink and its preparation method provided in this example are roughly the same as those in Example 1. The main difference is that the binder was not modified by transesterification.
[0025] Comparative Example 2: The environmentally friendly plant-based odor-free quick-drying ink and its preparation method provided in this example are largely the same as those in Example 1, except that castor oil-based acrylate is not added to the raw materials.
[0026] Comparative Example 3: The environmentally friendly plant-based deodorizing and quick-drying ink and its preparation method provided in this example are roughly the same as those in Example 1. The main difference is that vacuum distillation was not performed in step one to remove low-boiling-point odor components.
[0027] Performance testing and results analysis The inks prepared in Examples 1-4 and Comparative Examples 1-3 were subjected to performance tests, and the relevant data were recorded in Tables 1 and 2.
[0028] (1) Environmental performance testing: VOC content: Gas chromatography (GB / T23986-2009); Heavy metal content: ICP-MS detection of lead, mercury, cadmium, and hexavalent chromium (GB24613-2009).
[0029] (2) Drying performance test: Surface drying time: Finger touch method (GB / T1728-1979), record the time when the ink surface is no longer sticky to the touch; Drying time: Filter paper method (GB / T1728-1979), record the time for complete curing of ink.
[0030] Table 1: Experimental Data Recording Table
[0031] (3) Printability testing: Viscosity: Rotational viscometer (25℃, 60rpm, GB / T10247-2008); Gloss: Gloss meter (60° angle, GB / T9754-2007).
[0032] (4) Odor neutralization performance: Odor residues: GC-MS was used to detect the content of aldehydes and ketones; Sensory evaluation: 5-person group rating (1-5, level 1 no odor, level 5 strong odor).
[0033] (5) Storage stability: Viscosity change rate: The percentage change in viscosity is measured after storage at 40℃ for 30 days. Sedimentation and stratification: Observe whether stratification occurs after the ink has been left to stand for 90 days.
[0034] Table 2: Experimental Data Recording Table
[0035] As shown in Tables 1 and 2, compared with the comparative examples, the surface drying time of the inks prepared in Examples 1-4 is controlled within 10-15 minutes, and the actual drying time is ≤2 hours, demonstrating superior drying performance and meeting the requirements of high-efficiency printing. The odor level is only 1.0-1.5 (close to odorless), and the aldehyde residue is ≤4ppm, showing outstanding odor-neutralizing effect and meeting the requirements of high-end scenarios. The ink viscosity is stable at 600-900mPa・s, and the fineness is 10-15μm, resulting in uniform transfer and no particle feel during printing, with more stable printability and ensuring printing quality. The VOC content of Examples 1-4 is ≤15g / L, and the bio-based content is ≥92%, making the inks more environmentally friendly and in line with the green development trend. After storage at 40℃ for 30 days, the ink viscosity change rate is only +5.9% to +7.8%, and there is no sedimentation after 90 days, demonstrating stronger storage stability and extending shelf life.
[0036] This invention optimizes the molecular structure of vegetable oils through transesterification, and combines the synergistic effect of cobalt isooctanoate drier and castor oil-based acrylate to accelerate oxidative crosslinking and double bond polymerization, thereby improving drying efficiency and significantly increasing the turnover speed of printing production lines. Low-boiling-point odor substances in the vegetable oil are removed by vacuum distillation, and the low-odor drier cobalt isooctanoate controls odor at its source. It can be directly used in odor-sensitive applications such as food packaging and children's books. Transesterification modification makes the viscosity of the binder more suitable for the printing process, and the sufficient addition of carboxylated cellulose nanocrystals ensures uniform pigment dispersion. Castor oil-based acrylate improves film smoothness and guarantees the appearance quality of printed products. By using plant-based raw materials, the transesterification reaction reduces solvent dependence, and the deodorization and post-treatment processes produce no additional pollutant emissions.
[0037] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. An environmentally friendly, plant-based, odor-free, quick-drying ink, characterized in that... It contains the following raw materials in parts by weight: 20-28 parts pigment powder, 55-65 parts binder, 1.5-3 parts dispersant, 0.1-0.3 parts drier, 0.1-0.25 parts defoamer, 1-2 parts castor oil-based acrylate and 1-5 parts di-tert-butyl-p-cresol; The binder is made from the following raw materials: 45-50 parts flaxseed oil, 15-20 parts castor oil, 25-30 parts soybean oil, 20-30 parts methanol, and 0.5-1 parts potassium hydroxide.
2. The environmentally friendly plant-based odor-free and quick-drying ink according to claim 1, characterized in that: The pigment powder is selected from any one of phthalocyanine blue, phthalocyanine red, and iron oxide yellow.
3. The environmentally friendly plant-based odor-free and quick-drying ink according to claim 1, characterized in that: The dispersant is selected from carboxylated cellulose nanocrystals.
4. The environmentally friendly plant-based odor-free and quick-drying ink according to claim 1, characterized in that: The drying agent is selected from either cobalt isooctanoate or manganese isooctanoate.
5. A method for preparing an environmentally friendly, plant-based, odor-free, quick-drying ink, characterized in that, The preparation of the environmentally friendly plant-based odor-free and quick-drying ink according to any one of claims 1-4 includes the following steps: I. Raw material pretreatment: Weigh flaxseed oil, soybean oil and castor oil, and vacuum dehydrate and vacuum distill to remove low-boiling-point odor components, then mix them for later use. Weigh pigment powder, dispersant, drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol separately, and vacuum calcine the pigment powder and cool it for later use. II. Preparation of binder: Add the dehydrated mixed vegetable oil to the reactor and start stirring at a speed of 200-300 r / min. During stirring, slowly add methanol and potassium hydroxide dropwise to the reactor. After the addition is complete, raise the reactor temperature to 60-65℃ and react at a constant temperature for 2-3 hours. Take samples every 30 minutes to test the acid value. When the acid value stabilizes below 5 mg KOH / g, stop the reaction. Post-process the product to obtain the transesterification modified binder. III. Pigment Dispersion Treatment: Place the prepared transesterification modified binder into a stirring container, evacuate to -0.08 to -0.1 MPa, and slowly add the treated pigment powder and dispersant while stirring at a speed of 500-800 r / min. Stir for 30 to 60 minutes to initially disperse the pigment. Then, send it to a three-roll mill, control the grinding temperature at 40 to 50°C, and simultaneously purge nitrogen to grind until the ink fineness reaches 10 to 15 μm. IV. Ink Preparation: Place the ground material into a mixing container, vacuum to -0.08 to -0.1 MPa, add drier, defoamer, castor oil-based acrylate and di-tert-butyl-p-cresol, and stir at 300-500 r / min for 20-40 minutes to ensure uniform dispersion of the additives before discharging to obtain ink. V. The finished ink is degassed by a vacuum degassing machine to remove microbubbles and impurities are removed by a precision filter to obtain the finished ink. The ink is then filled into aluminum cans under nitrogen cover and stored in a sealed, light-proof container.
6. The method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink according to claim 5, characterized in that, In step I, the flaxseed oil, soybean oil and castor oil are mixed in a ratio of 5:3:2 and stirred for 30 minutes under vacuum of -0.09 MPa and temperature of 60°C to dehydrate the mixture and control the moisture content to below 0.1%.
7. The method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink according to claim 5, characterized in that, In step I, the pigment powder is calcined at a high temperature of 500-800℃ for 2-4 hours to remove adsorbed organic impurities and volatile odor substances from the surface.
8. The method for preparing an environmentally friendly plant-based, odor-free, quick-drying ink according to claim 5, characterized in that, In step II, the post-processing of the product includes the following steps: A1. Neutralization and Deacidification: Cool the reaction product to below 40℃, slowly add a 5% (w / w) phosphoric acid solution, stir for 30 minutes, adjust the pH to 6-7, allow to stand and separate into layers, then remove the lower aqueous phase. A2. Water washing and purification: Add 20% (by mass) of deionized water to the product generated by the neutralization reaction, stir at 50°C for 20 minutes, allow to stand and separate into layers, remove the lower aqueous phase, and repeat water washing until the pH of the aqueous phase stabilizes at 6.9-7.
1. A3. Dehydration and drying: Place the washed product into a rotary evaporator and distill for 30 minutes under a vacuum of -0.09 MPa and a temperature of 70°C to remove residual methanol and water. A4. Filtration and purification: The dried product is filtered through an organic filter membrane with a pore size of 0.22μm to obtain a clear and transparent transesterification modified binder.