Color paste for gel pen ink and preparation method of color paste
By using a color paste of a specific composition in the gel pen ink and using a dispersant synthesized from materials such as polyacrylic acid, the problem of easy aggregation or precipitation of pigment particles in the existing purple gel pen ink is solved, and the stability of the color paste is significantly improved. and weather resistance, improving ink quality and usage experience.
Patent Information
- Application Number
- CN202411507139.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-28
- Publication Date
- 2025-01-21
AI Technical Summary
The color paste in existing purple neutral pen ink is easy to accumulate or precipitate due to pigment particles, resulting in uneven color of the ink after long-term storage, affecting the overall quality and user experience of the neutral pen ink.
A gel pen ink color paste is used, and its composition includes 15 to 22 parts of pigment, 3 to 6 parts of wetting agent, 8 to 12 parts of dispersant, 0.1 to 0.5 parts of defoaming agent, 8 to 15 parts of cosolvent, 45 to 60 parts water, through specific dispersant preparation methods, including polypropylene Synthesis of olefinic acid, sodium alginate, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide, N-hydroxysuccinimide, chitosan, and methyl methacrylate to reduce purple color The mutual attraction between pigments prevents aggregation and prevents particle settling through a suspended network structure.
It significantly improves the stability and weather resistance of the color paste, avoids problems such as precipitation of pigment particles and uneven color, and improves the overall quality and use experience of gel pen ink.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of color paste, and in particular to a color paste for gel pen ink and a preparation method thereof. Background Art
[0002] Currently, there are many types of gel pen inks on the market, and purple ink is widely used in writing, painting, and marking due to its unique color.
[0003] However, the pigment paste in existing purple inks often aggregates or precipitates easily, resulting in uneven color after long-term storage. Currently, there are relatively few studies on the preparation and performance optimization of purple color pastes, which affects the overall quality and user experience of neutral pen inks.
[0004] In view of this, this application is filed. Summary of the invention
[0005] The invention provides a color paste for gel pen ink and a preparation method thereof. The color paste of the invention has excellent stability and excellent weather resistance and has broad application prospects.
[0006] The present invention solves the technical problem by adopting the following technical solutions: A color paste for gel pen ink comprises the following components in parts by weight: 15 to 22 parts of pigment, 3 to 6 parts of wetting agent, 8 to 12 parts of dispersant, 0.1 to 0.5 parts of defoaming agent, 8 to 15 parts of cosolvent and 45 to 60 parts of water.
[0007] As a preferred embodiment of the present invention, the structural formula of the pigment is as shown in Formula I: .
[0008] As a preferred embodiment of the present invention, the method for preparing the dispersant comprises the following steps: (1) Add polyacrylic acid, sodium alginate and butyl acetate into water, stir evenly, then add 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide, stir evenly to obtain a precursor; (2) Add chitosan, methyl methacrylate, initiator and mercaptoethanol to the precursor, react at 65-75°C for 2-5 hours, ultrasonically treat, and rotary evaporate to remove the solvent to obtain a dispersant.
[0009] The dispersant of the present invention is synthesized from polyacrylic acid, sodium alginate, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide, N-hydroxysuccinimide, chitosan and methyl methacrylate under the action of an auxiliary agent. The polyacrylic acid (excessive, the excess provides enough carboxyl groups, part of the carboxyl groups react, and part of the carboxyl groups are retained), wherein part of the carboxyl groups react with methyl methacrylate, thereby reducing the mutual attraction between purple pigments, avoiding aggregation, increasing the static electricity or steric hindrance on the surface of the purple pigment, thereby improving stability, and part of the carboxyl groups react with chitosan to form a suspended network structure to prevent particle sedimentation and improve system viscosity. The dispersant of the present invention has excellent compatibility with the purple pigment of the present invention, can effectively improve the dispersibility and stability of the purple pigment, and improve weather resistance.
[0010] Wherein, the polyacrylic acid mentioned in the present invention is conventional polyacrylic acid in the art.
[0011] Exemplarily, the polyacrylic acid is polyacrylic acid with a grade of CY-D2 provided by Changyao Chemical.
[0012] As a preferred embodiment of the present invention, the mass ratio of the polyacrylic acid, sodium alginate, butyl acetate, water, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide is 100:(8-12):(40-100):(300-600):(4-10):(4-10).
[0013] As a preferred embodiment of the present invention, the mass ratio of the polyacrylic acid, chitosan, methyl methacrylate, initiator and mercaptoethanol is 100: (10-20): (8-15): (2-6): (2-6).
[0014] As a preferred embodiment of the present invention, the initiator is at least one of azobisisobutyronitrile, azobisisoheptanenitrile, benzoyl peroxide, and dicumyl peroxide.
[0015] As a preferred embodiment of the present invention, the power of the ultrasonic treatment is 500-800 W, and the time is 25-50 min.
[0016] As a preferred embodiment of the present invention, the wetting agent is sodium dioctyl sulfonate dibutyrate; The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1: (0.5-2).
[0017] As a preferred embodiment of the present invention, the cosolvent is at least one of ethylene glycol, propylene glycol, glycerol, diethylene glycol, and polyethylene glycol; The defoaming agent is a silicone defoaming agent.
[0018] The present invention also provides a method for preparing a color paste for gel pen ink, comprising the following steps: Add dispersant, wetting agent and co-solvent into water, stir evenly at a speed of 400-700 rpm, add pigment, stir evenly at a speed of 800-1200 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at a speed of 200-500 rpm to obtain a color paste for gel pen ink.
[0019] The beneficial effects of the present invention are as follows: the dispersant of the present invention is synthesized from polyacrylic acid, sodium alginate, 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide, N-hydroxysuccinimide, chitosan and methyl methacrylate under the action of an auxiliary agent; the polyacrylic acid (excessive, the excess provides enough carboxyl groups, part of the carboxyl groups react, and part of the carboxyl groups are retained), wherein part of the carboxyl groups react with methyl methacrylate, thereby reducing the mutual attraction between purple pigments, avoiding aggregation, increasing the static electricity or steric hindrance on the surface of the purple pigment, thereby improving stability; part of the carboxyl groups react with chitosan to form a suspended network structure to prevent particle sedimentation and improve system viscosity; the dispersant of the present invention has excellent compatibility with the purple pigment of the present invention, can effectively improve the dispersibility and stability of the purple pigment, and improve weather resistance. DETAILED DESCRIPTION
[0020] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0021] In the present invention, the technical features described in an open manner include closed technical solutions composed of the listed features, and also include open technical solutions containing the listed features.
[0022] In the present invention, when it comes to numerical ranges, unless otherwise specified, the above numerical ranges are deemed to be continuous and include the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges included therein.
[0023] In the present invention, there is no particular limitation on the specific dispersion and stirring treatment methods.
[0024] The reagents or instruments used in the present invention without indicating the manufacturer are all conventional products that can be obtained commercially. The raw materials used in the comparative examples and the raw materials used in the parallel experiments of the embodiments are the same commercially available products unless otherwise specified.
[0025] Example 1 A color paste for gel pen ink comprises the following components in parts by weight: 20 parts of pigment, 5 parts of wetting agent, 10 parts of dispersant, 0.3 parts of defoaming agent, 12 parts of propylene glycol and 52.7 parts of water.
[0026] The wetting agent is sodium dioctyl sulfonate dibutyrate.
[0027] The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1:1.
[0028] The defoamer is BYK1790.
[0029] The structural formula of the pigment is shown in Formula I: .
[0030] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 8 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 8 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 15 parts of chitosan, 12 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0031] The method for preparing the color paste for gel pen ink comprises the following steps: Add dispersant, wetting agent and propylene glycol into water, stir evenly at 500 rpm, add pigment, stir evenly at 1000 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at 400 rpm to obtain a color paste for gel pen ink.
[0032] Example 2 A color paste for gel pen ink comprises the following components in parts by weight: 15 parts of pigment, 6 parts of wetting agent, 8 parts of dispersant, 0.5 parts of defoaming agent, 15 parts of propylene glycol and 55.5 parts of water.
[0033] The wetting agent is sodium dioctyl sulfonate dibutyrate.
[0034] The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1:1.
[0035] The defoamer is BYK1790.
[0036] The structural formula of the pigment is shown in Formula I: .
[0037] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 8 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 8 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 15 parts of chitosan, 12 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0038] The method for preparing the color paste for gel pen ink comprises the following steps: Add dispersant, wetting agent and propylene glycol into water, stir evenly at 500 rpm, add pigment, stir evenly at 1000 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at 400 rpm to obtain a color paste for gel pen ink.
[0039] Example 3 A color paste for gel pen ink comprises the following components in parts by weight: 22 parts of pigment, 3 parts of wetting agent, 12 parts of dispersant, 0.1 parts of defoaming agent, 8 parts of propylene glycol and 54.9 parts of water.
[0040] The wetting agent is sodium dioctyl sulfonate dibutyrate.
[0041] The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1:1.
[0042] The defoamer is BYK1790.
[0043] The structural formula of the pigment is shown in Formula I: .
[0044] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 8 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 8 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 15 parts of chitosan, 12 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0045] The method for preparing the color paste for gel pen ink comprises the following steps: Add dispersant, wetting agent and propylene glycol into water, stir evenly at 500 rpm, add pigment, stir evenly at 1000 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at 400 rpm to obtain a color paste for gel pen ink.
[0046] Example 4 A color paste for gel pen ink comprises the following components in parts by weight: 20 parts of pigment, 5 parts of wetting agent, 10 parts of dispersant, 0.3 parts of defoaming agent, 12 parts of propylene glycol and 52.7 parts of water.
[0047] The wetting agent is sodium dioctyl sulfonate dibutyrate.
[0048] The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1:1.
[0049] The defoamer is BYK1790.
[0050] The structural formula of the pigment is shown in Formula I: .
[0051] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 8 parts of sodium alginate, and 100 parts of butyl acetate to 300 parts of water, stir at 500 rpm, then add 4 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 4 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 10 parts of chitosan, 15 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0052] The method for preparing the color paste for gel pen ink comprises the following steps: Add dispersant, wetting agent and propylene glycol into water, stir evenly at 500 rpm, add pigment, stir evenly at 1000 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at 400 rpm to obtain a color paste for gel pen ink.
[0053] Example 5 A color paste for gel pen ink comprises the following components in parts by weight: 20 parts of pigment, 5 parts of wetting agent, 10 parts of dispersant, 0.3 parts of defoaming agent, 12 parts of propylene glycol and 52.7 parts of water.
[0054] The wetting agent is sodium dioctyl sulfonate dibutyrate.
[0055] The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1:1.
[0056] The defoamer is BYK1790.
[0057] The structural formula of the pigment is shown in Formula I: .
[0058] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 12 parts of sodium alginate, and 40 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 10 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 10 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 20 parts of chitosan, 8 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0059] The method for preparing the color paste for gel pen ink comprises the following steps: Add dispersant, wetting agent and propylene glycol into water, stir evenly at 500 rpm, add pigment, stir evenly at 1000 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at 400 rpm to obtain a color paste for gel pen ink.
[0060] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that the preparation method of the dispersant is different, and the other aspects are the same.
[0061] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, and stir at 500 rpm to obtain a precursor; (2) Add 15 parts of chitosan, 12 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0062] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the preparation method of the dispersant is different, and the other aspects are the same.
[0063] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 8 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 8 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 12 parts of methyl methacrylate, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600 W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0064] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the preparation method of the dispersant is different, and the other aspects are the same.
[0065] The preparation method of the dispersant (parts in the preparation process are all parts by weight) comprises the following steps: (1) Add 100 parts of polyacrylic acid, 10 parts of sodium alginate, and 60 parts of butyl acetate to 600 parts of water, stir at 500 rpm, then add 8 parts of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 8 parts of N-hydroxysuccinimide, stir at 500 rpm to obtain a precursor; (2) Add 15 parts of chitosan, 5 parts of azobisisobutyronitrile and 5 parts of mercaptoethanol to the precursor of step (1), react at 70°C for 4 hours, ultrasonically treat at 600W for 40 minutes, and remove the solvent by rotary evaporation to obtain a dispersant.
[0066] Test Case 1. Stability test (1) Sedimentation rate: The test was conducted using the LUMISIZER611 high-speed centrifuge stabilizer manufactured by LUMISIZER of Germany according to the instructions. Specifically, the wavelength of the test light source was 865 nm, the rotation speed was 4000 r / min, the interval was 30 s, the number of scans was 1000, and the test temperature was room temperature.
[0067] (2) Stability: The color pastes prepared in the examples and comparative examples were placed at 25° C. for 180 days, and the stability of the pigment color pastes was determined by visually observing whether there was obvious precipitation, flocculation, stratification, or agglomeration of pigment particles.
[0068] 2. The weather resistance of the prepared color paste was tested by artificial accelerated aging method using QUV (ultraviolet light). The color difference (ΔE) before and after accelerated aging irradiation was measured by X-rite portable spectrophotometer. QUV (ultraviolet light) accelerated aging was performed for 1000 hours.
[0069] Table 1
[0070] It can be seen from Table 1 that the color paste of the present invention has excellent stability and excellent weather resistance, and has broad application prospects.
[0071] By comparing Example 1 with Comparative Example 1, it can be seen that the dispersant prepared by the present invention can significantly improve the stability and weather resistance of the color paste, and the dispersants prepared by different methods have different improvements in stability and weather resistance. The dispersant prepared by the method of the present invention has better compatibility with the purple pigment, and can more significantly improve the stability and weather resistance compared to the dispersants prepared by other methods.
[0072] Finally, it should be noted that the above embodiments are intended to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.
Claims
1. A color paste for gel pen ink, characterized in that: The invention comprises the following components in parts by weight: 15 to 22 parts of pigment, 3 to 6 parts of wetting agent, 8 to 12 parts of dispersant, 0.1 to 0.5 parts of defoaming agent, 8 to 15 parts of cosolvent and 45 to 60 parts of water.
2. The gel pen ink paste according to claim 1, characterized in that: The structural formula of the pigment is shown in Formula I: 。 3. The gel pen ink paste according to claim 1, characterized in that: The preparation method of the dispersant comprises the following steps: (1) Add polyacrylic acid, sodium alginate and butyl acetate into water, stir evenly, then add 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide, stir evenly to obtain a precursor; (2) Add chitosan, methyl methacrylate, initiator and mercaptoethanol to the precursor, react at 65-75°C for 2-5 hours, ultrasonically treat, and rotary evaporate to remove the solvent to obtain a dispersant.
4. The gel pen ink paste according to claim 3, characterized in that: The mass ratio of the polyacrylic acid, sodium alginate, butyl acetate, water, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and N-hydroxysuccinimide is 100:(8-12):(40-100):(300-600):(4-10):(4-10).
5. The gel pen ink paste according to claim 3, characterized in that: The mass ratio of the polyacrylic acid, chitosan, methyl methacrylate, initiator and mercaptoethanol is 100: (10-20): (8-15): (2-6): (2-6).
6. The gel pen ink paste according to claim 3, characterized in that: The initiator is at least one of azobisisobutyronitrile, azobisisoheptanenitrile, benzoyl peroxide and dicumyl peroxide.
7. The gel pen ink paste according to claim 3, characterized in that: The power of the ultrasonic treatment is 500-800W, and the time is 25-50min.
8. The gel pen ink paste according to claim 1, characterized in that: The wetting agent is sodium dioctyl sulfonate dibutyrate; The dispersant is a mixture of n-octanol polyoxyethylene ether and Tween 60, and the mass ratio of n-octanol polyoxyethylene ether to Tween 60 is 1: (0.5-2).
9. The gel pen ink paste according to claim 1, characterized in that: The cosolvent is at least one of ethylene glycol, propylene glycol, glycerol, diethylene glycol, and polyethylene glycol; The defoaming agent is a silicone defoaming agent.
10. The method for preparing a gel pen ink paste according to any one of claims 1 to 9, characterized in that: The following steps are involved: Add dispersant, wetting agent and co-solvent into water, stir evenly at a speed of 400-700 rpm, add pigment, stir evenly at a speed of 800-1200 rpm to obtain a mixture; grind the mixture with a sand mill to a particle size of less than 0.25 μm, add defoamer, stir evenly at a speed of 200-500 rpm to obtain a color paste for gel pen ink.