Ink and preparation process thereof

By using graphite ore to prepare ink, combined with the synergistic effect of aging and composite bile, the problems of traditional ink in precipitation, mold, blackness distortion and insufficient gloss are solved, and the preparation of high-quality ink is achieved, which significantly improves the weather resistance of ink traces.

CN119955349APending Publication Date: 2025-05-09SHEXIAN JIYA MO FACTORY
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Patent Information

Application Number
CN202510208033.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-25
Publication Date
2025-05-09

AI Technical Summary

Technical Problem

Traditional inks are prone to precipitation, mold, inauthentic blackness and poor brightness during use, which is difficult to meet the cultural market's demand for high-quality ink.

Method used

Graphite ore is used as the black raw material, and graphite powder is pressed and rinsed, dried, aged, etc., combined with gelatin, auxiliary materials, water, grease, borneol and artificial musk, and heat-raising stirring, maturation, steaming and rolling, high-quality ink is prepared.

Benefits of technology

It significantly improves the anti-precipitation, anti-mold, blackness and brightness performance of the ink, and the weather resistance of the ink mark can reach more than 5 times that of ordinary ink.

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Abstract

The invention discloses ink and a preparation process thereof, and belongs to the technical field of ink production.The preparation process of the ink comprises the following steps that graphite ore is taken and pressed into graphite powder, pure graphite powder is obtained through rinsing and drying, cured graphite powder is obtained through aging, and the pure graphite powder and the cured graphite powder are mixed; the preparation method comprises the following steps: mixing cured graphite powder, gelatin, auxiliary materials, water, grease, borneol and artificial musk according to a dosage ratio, heating and stirring until the mixture is muddy to obtain ink mud, preparing the ink mud into an ink cake while the ink mud is hot, curing, steaming and rolling, adding pure water according to a solid-to-liquid ratio of 1: (0.3-0.4), and stirring and mixing to obtain the ink. The graphite ore is used for preparing the ink, and through detection, the settling velocity, the mildew-proof grade, the blackness and the glossiness of the finally prepared ink are all remarkably improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of ink production, and in particular relates to ink and a preparation process thereof. Background Art

[0002] With the development of science and technology, the scope of use of Hui ink is getting smaller and smaller, and the Chinese ink-making craft that has been passed down for thousands of years is on the verge of extinction. As the traditional ink-making craft is selected into the "intangible cultural heritage" protection list, this itself shows that the prospects of traditional ink-making craft are worrying. As more and more people love calligraphy and painting in Chinese culture, from a pragmatic point of view, ink can occupy a place in the cultural market.

[0003] Ink seems to be easy to use, but the process varies greatly and the materials used are different, which leads to some problems for users: precipitation, mold, false blackness and poor brightness. In order to overcome these weaknesses, the present invention provides an authentic ink, which uses natural graphite ore as the black raw material to make "graphite ink". Summary of the invention

[0004] The object of the present invention is to provide an ink and a preparation process thereof, aiming to improve the anti-precipitation performance, mildew resistance, blackness and brightness performance of the prepared ink.

[0005] The purpose of the present invention can be achieved by the following technical solutions: A process for preparing ink comprises the following steps: Graphite ore is pressed into graphite powder, which is then rinsed and dried to obtain pure graphite powder, which is then aged to obtain matured graphite powder. The matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk are mixed according to the usage ratio, and the temperature is increased and stirred until it becomes a mud-like state to obtain ink mud. The ink mud is made into ink cake while it is hot, and after aging, steaming and rolling, pure water is added into the mixture according to the solid-liquid ratio of 1:0.3-0.4, and the mixture is stirred and mixed to obtain ink.

[0006] Furthermore, the graphite powder includes the following components: 81.7% to 85.1% graphite, 2.8% to 5.4% quartz, 1.1% to 3.5% muscovite, 1.5% to 3.2% biotite, 0.5% to 1.7% potassium feldspar, 0.5% to 1.0% plagioclase, 0.4% to 0.7% kaolinite, 0.2% to 0.5% montmorillonite, 0.1% to 1% pyrite, and other unmeasurable impurities and moisture.

[0007] Furthermore, the auxiliary material is compounded by bile, flavor liquid, blackening agent and stabilizer in a mass ratio of 3-8:5-10:10-15:1-3.

[0008] Furthermore, the bile is compounded from pig bile, chicken bile, bear bile and snake bile in a volume ratio of 1:1:0.01 to 0.1:0.5.

[0009] Furthermore, the spice liquid is prepared by mixing cloves, cinnamon, ash bark, sandalwood and gamboge in a mass ratio of 5-6:4-5:3-4:3-4:1-2, and then crushing, boiling and filtering.

[0010] Furthermore, the raw material of the gelatin is prepared by mixing buffalo hide, cattle hide, ox horn, fish skin and donkey hide in a mass ratio of 20:20:3-4:5-10:2-4 and then boiling.

[0011] Furthermore, the usage ratio of the cooked graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk is 350g:110-120g:70-80g:350-400mL:2g:2g:0.8-1.0g.

[0012] Furthermore, the ink is prepared by the above preparation process.

[0013] Beneficial effects of the present invention: The present invention provides a process for preparing ink. Different from the prior art of producing ink using carbon black, the present invention uses graphite ore to prepare ink. After testing, the sedimentation rate, mildew resistance level, blackness and glossiness of the ink finally prepared are significantly improved. The specific principle is as follows: Anti-precipitation performance: The carbon black particles of traditional carbon black ink have low surface polarity, are easy to agglomerate and settle, need to be frequently shaken, have poor colloidal stability, and have obvious stratification after long-term storage. The present invention uses graphite powder to prepare ink, which contains quartz (SiO 2 ), muscovite and other layered silicates, which physically block particle sedimentation through the lamellar structure; at the same time, the present invention ages the pure graphite powder in the dark for 3 to 5 years. During the aging process, the hydroxyl groups on the surface of the pure graphite powder are oxidized to form hydrophilic groups (-OH, -COOH), which enhance the hydrogen bonding effect with water, thereby helping to reduce the probability of sedimentation problems in the final ink produced.

[0014] Anti-mildew performance: Traditional ink uses sodium benzoate as a preservative, which has toxic risks and a short anti-mildew period. The present invention uses composite bile active ingredients and flavor liquid to achieve synergistic anti-mildew. Specifically, the bile salts contained in pig / chicken bile in the composite bile can destroy the cell membranes of microorganisms such as molds, and the taurine in snake bile can inhibit the growth of Aspergillus flavus hyphae; at the same time, the cloves (active ingredient eugenol) + cinnamon (active ingredient cinnamaldehyde) in the flavor liquid have a synergistic antibacterial effect, ultimately achieving the purpose of improving the anti-mildew performance of the produced ink.

[0015] Blackness performance: The reflectivity of traditional carbon black ink to visible light (400-700nm) is about 5%-8%, and the blackness (L* value) is usually greater than 25. The graphite mineral ink prepared by the present invention uses graphite to provide the base blackness, and then adds manganese dioxide / manganese tetraoxide to fill the graphite lattice defects and enhance near-infrared absorption, thereby achieving the purpose of synergistic blackening. After testing, the blackness (L* value) of the ink produced by the present invention reaches 18-21 (the lower the value, the darker it is).

[0016] Brightness performance: Traditional carbon black has mainly diffuse reflection due to its porous surface, and the gloss (measured at an angle of 60°) is usually <10GU. The present invention utilizes the synergistic effect of borneol and oil in the ink to achieve the purpose of improving the gloss of the final prepared ink. Specifically, borneol (borneol) can reduce the surface tension of the ink, thereby promoting the leveling of the ink, and the oil can form a molecular-level film on the surface of the ink to improve the mirror reflectivity of the ink surface. Under the combined effect, the gloss of the final produced ink reaches 22 to 25GU.

[0017] Finally, the ink production process provided by the present invention solves the problems of precipitation, mildew, blackness distortion and insufficient gloss while maintaining the writing function of traditional ink through a mineral composite suspension system, a natural biological anticorrosion network, a manganese-based optical enhancement system, etc., and in particular, through the synergistic effect of 3 to 5 years of graphite aging and composite bile, a coupling effect of anticorrosion-blackening-suspension is achieved, and the weather resistance of the ink finally produced can reach more than 5 times that of ordinary ink. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only 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.

[0019] The present invention utilizes the high-quality graphite mine in Shimo Ridge, Yi County, Huangshan City, Anhui Province. A few years ago, the state built a high-speed railway through Shimo Ridge, and dug out the dormant graphite mine. The graphite mine was black and shiny, which awakened the Huizhou ink worker - Wu Jihei, who used the graphite mine as a black colorant. Historical data Yi County Chronicles records: Yuting Road in this county, on Shibali Ridge in the south of the county, there is a stone cave, in which there is soft and greasy graphite, which the master took as ink color and was very bright green, and could record words. Example 1

[0020] A process for preparing ink comprises the following steps: First, the above graphite ore is taken and pressed into powder to obtain graphite powder. After testing, the graphite powder includes the following components by mass percentage: 81.7% graphite, quartz (SiO2 ) 2.8%, muscovite 1.1%, biotite 1.5%, potassium feldspar 0.5%, plagioclase 0.5%, kaolinite 0.4%, montmorillonite 0.2%, pyrite (FeS 2 ) 0.1%, other unmeasurable impurities and moisture.

[0021] Then, the graphite powder was rinsed three times with clean water, and the washing slurry was collected to obtain graphite slurry, and the graphite slurry was then dried at 80° C. to constant weight to obtain pure graphite powder, and the pure graphite powder was then placed in a dry and light-proof environment for aging for 3 years to obtain matured graphite powder.

[0022] Next, the bile, the spice liquid, the blackening agent and the stabilizer are compounded in a mass ratio of 3:5:10:1 to obtain an auxiliary material. Among them, the bile is compounded by pig bile, chicken bile, bear bile and snake bile in a volume ratio of 1:1:0.01:0.5. The spice liquid is prepared by mixing cloves, cinnamon, ash bark, sandalwood and gamboge in a mass ratio of 5:4:3:3:1, crushing, boiling and filtering. Specifically, cloves, cinnamon, ash bark, sandalwood and gamboge are mixed in the above mass ratio and crushed through a 50-mesh sieve, and then pure water is added to it in a solid-liquid ratio of 1:4 and boiled. During the boiling process, it is kept in a slightly boiling state for 0.5h. After completion, it is cooled to room temperature and filtered with a 120-mesh filter to obtain a spice liquid. Among them, the blackening agent is manganese dioxide and the stabilizer is sodium bicarbonate.

[0023] Secondly, boil the gelatin. Specifically, the raw materials of gelatin are buffalo hide, cattle hide, ox horns, fish skin and donkey hide, which are mixed in a mass ratio of 20:20:3:5:2 and then boiled. The boiled gelatin needs to be aged in a light-proof and dry environment for five years. Adding the above gelatin is the key to preventing the ink from odor.

[0024] Again, the matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk are mixed in a dosage ratio of 350g:110g:70g:350mL:2g:2g:0.8g, placed in a blender and heated to 40°C, stirred at a constant temperature until it becomes a mud, taken out to obtain ink mud, and the ink mud is made into ink cakes while it is hot, and the ink cakes are placed in a light-proof environment and matured for 7 days. After completion, the matured ink cakes are placed in a steamer and steamed for 1 hour, and then placed in a three-roller mill and rolled 10 times, and then pure water is added to the rolled ink mud at a solid-liquid ratio of 1:0.3, and stirred and mixed evenly to obtain ink. Example 2

[0025] A process for preparing ink comprises the following steps: First, the above graphite ore is taken and pressed into powder to obtain graphite powder. After testing, the graphite powder includes the following components by mass percentage: 84.3% graphite, quartz (SiO 2) 3.3%, muscovite 2.0%, biotite 1.7%, potassium feldspar 1.0%, plagioclase 0.7%, kaolinite 0.5%, montmorillonite 0.3%, pyrite (FeS 2 ) 0.4%, other undetectable impurities and moisture.

[0026] Then, the graphite powder was rinsed three times with clean water, and the washing slurry was collected to obtain graphite slurry, and the graphite slurry was then dried at 100° C. to constant weight to obtain pure graphite powder, and the pure graphite powder was then placed in a dry and light-proof environment for aging for 5 years to obtain matured graphite powder.

[0027] Next, the bile, the spice liquid, the blackening agent and the stabilizer are compounded in a mass ratio of 5:7:11:2 to obtain an auxiliary material. Among them, the bile is compounded by pig bile, chicken bile, bear bile and snake bile in a volume ratio of 1:1:0.04:0.5. The spice liquid is prepared by mixing cloves, cinnamon, ash bark, sandalwood and gamboge in a mass ratio of 6:4:4:4:2, crushing, boiling and filtering. Specifically, cloves, cinnamon, ash bark, sandalwood and gamboge are mixed in the above mass ratio and crushed through a 50-mesh sieve, and then pure water is added to it in a solid-liquid ratio of 1:4.5 and boiled. During the boiling process, it is kept in a slightly boiling state for 1.0h. After completion, it is cooled to room temperature and filtered with a 120-mesh filter to obtain a spice liquid. Among them, the blackening agent is manganese tetraoxide and the stabilizer is sodium bicarbonate.

[0028] Secondly, boil the gelatin. Specifically, the raw materials of gelatin are buffalo hide, cattle hide, ox horns, fish skin and donkey hide, which are mixed in a mass ratio of 20:20:4:8:3 and then boiled. The boiled gelatin needs to be aged in a light-proof and dry environment for five years. Adding the above gelatin is the key to preventing the ink from odor.

[0029] Again, the matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk are mixed in a dosage ratio of 350g:120g:75g:350mL:2g:2g:1.0g, placed in a blender and heated to 45°C, stirred at a constant temperature until it becomes a mud, taken out to obtain ink mud, and the ink mud is made into ink cakes while it is hot, and the ink cakes are placed in a light-proof environment and matured for 7 days. After completion, the matured ink cakes are placed in a steamer and steamed for 2 hours, and then placed in a three-roller mill and rolled 20 times, and then pure water is added to the rolled ink mud at a solid-liquid ratio of 1:0.35, and stirred and mixed evenly to obtain ink. Example 3

[0030] A process for preparing ink comprises the following steps: First, the above graphite ore is taken and pressed into powder to obtain graphite powder. After testing, the graphite powder includes the following components by mass percentage: 85.1% graphite, quartz (SiO 2) 5.4%, muscovite 3.5%, biotite 3.2%, potassium feldspar 1.7%, plagioclase 1.0%, kaolinite 0.7%, montmorillonite 0.5%, pyrite (FeS 2 ) 1%, other undetectable impurities and moisture.

[0031] Then, the graphite powder was rinsed three times with clean water, and the washing slurry was collected to obtain graphite slurry, and the graphite slurry was then dried at 100° C. to constant weight to obtain pure graphite powder, and the pure graphite powder was then placed in a dry and light-proof environment for aging for 5 years to obtain matured graphite powder.

[0032] Next, bile, spice liquid, blackening agent and stabilizer are compounded in a mass ratio of 8:10:15:3 to obtain auxiliary materials. Among them, bile is compounded by pig bile, chicken bile, bear bile and snake bile in a volume ratio of 1:1:0.1:0.5. The spice liquid is prepared by mixing cloves, cinnamon, ash bark, sandalwood and gamboge in a mass ratio of 6:5:4:4:2, crushing, boiling and filtering. Specifically, cloves, cinnamon, ash bark, sandalwood and gamboge are mixed in the above mass ratio and crushed through a 50-mesh sieve, and then pure water is added to it in a solid-liquid ratio of 1:5 and boiled. During the boiling process, it is kept in a slightly boiling state for 1.0h. After completion, it is cooled to room temperature and filtered with a 120-mesh filter to obtain a spice liquid. Among them, the blackening agent is manganese tetraoxide and the stabilizer is sodium bicarbonate.

[0033] Secondly, boil the gelatin. Specifically, the raw materials of gelatin are buffalo hide, cattle hide, ox horns, fish skin and donkey hide, which are mixed in a mass ratio of 20:20:4:10:4 and then boiled. The boiled gelatin needs to be aged in a light-proof and dry environment for five years. Adding the above gelatin is the key to preventing the ink from odor.

[0034] Again, the matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk are mixed in a dosage ratio of 350g:120g:80g:400mL:2g:2g:1g, placed in a blender and heated to 50°C, stirred at a constant temperature until it becomes a mud-like state, taken out to obtain ink mud, and the ink mud is made into ink cakes while it is hot, and the ink cakes are placed in a light-proof environment and matured for 7 days. After completion, the matured ink cakes are placed in a steamer and steamed for 2 hours, and then placed in a three-roller mill and rolled 20 times, and then pure water is added to the rolled ink mud at a solid-liquid ratio of 1:0.4, and after stirring and mixing evenly, ink is obtained.

[0035] Comparative Example 1 Carbon black ink (purchased from Beijing Yidege Ink Industry Co., Ltd.).

[0036] The inks in Examples 1 to 3 and Comparative Example 1 were subjected to performance tests. The performance test process is as follows, and the test results are shown in Table 1: (1) Sedimentation rate (mm / day): Test standard: Refer to ASTM D869 (Standard for Determination of Coating Sedimentation).

[0037] Test process: After shaking the ink thoroughly, fill it into a 100mL stoppered measuring cylinder to the scale line, and place it vertically in a constant temperature (25±1℃) and light-proof environment for 30 days. Measure the thickness of the sedimentation layer with a vernier caliper every day (accurate to 0.1mm), and calculate the average daily sedimentation rate: sedimentation rate (mm / day) = total sedimentation thickness / number of days of standing.

[0038] (2) Mildew resistance level (ISO 846): Test standard: ISO 846 "Evaluation of the behavior of plastics under the action of fungi and bacteria".

[0039] Test process: Use mixed spore suspension (containing 1×10 6 CFU / mL±5% of Aspergillus niger, Penicillium, Chaetomium globosum, Aureobasidium bracteata, Paecilomyces variotii, Trichoderma viride, Penicillium funiculosum and Aspergillus terreus), the ink was applied to the filter paper, and the spraying amount of bacteria was 1×10 6 CFU / mL of suspension.

[0040] Culture conditions: temperature 28±2℃, humidity 90%, culture for 28 days.

[0041] Grade determination: Grade 0: no visible growth (complete inhibition); Grade 1: growth area <10%; Grade 2: growth area 10% to 30%; Grade 3: growth area >30%.

[0042] (3) Blackness L* value: Test standard: ISO 11664-4 (colorimetry standard).

[0043] Test process: Apply the ink evenly on standard white cardboard with a dry film thickness of 20±2μm. Use a spectrophotometer (model X-Rite Ci64) to measure under D65 light source and 10° observation angle. Record the lightness value L* in the CIE-Lab system (0 is pure black and 100 is pure white). Measure 5 points for each sample and take the average value. The standard deviation must be less than 0.5.

[0044] (4) Glossiness GU (60°): Test standard: ASTM D523 (specular gloss test standard).

[0045] Test process: The ink is applied to the glass plate with a dry film thickness of 15±1μm. The surface is smooth and scratch-free. The gloss meter is calibrated using a standard plate (high gloss plate GU=100, low gloss plate GU=10). Five different areas are measured at an incident angle of 60°, and the average value is taken. The reporting unit is GU (Gloss Unit). The higher the value, the stronger the gloss.

[0046] Table 1 Test results

[0047] It should be noted that, in this article, terms such as "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or equipment that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or equipment.

[0048] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A process for preparing ink, characterized in that: The following steps are involved: Graphite ore is pressed into graphite powder, which is then rinsed and dried to obtain pure graphite powder, which is then aged to obtain matured graphite powder. The matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk are mixed according to the usage ratio, and the temperature is increased and stirred until it becomes a mud-like state to obtain ink mud. The ink mud is made into ink cake while it is hot, and after aging, steaming and rolling, pure water is added into the mixture according to the solid-liquid ratio of 1:0.3-0.4, and the mixture is stirred and mixed to obtain ink.

2. The process for preparing ink according to claim 1, characterized in that: The graphite powder comprises the following components: 81.7% to 85.1% of graphite, 2.8% to 5.4% of quartz, 1.1% to 3.5% of muscovite, 1.5% to 3.2% of biotite, 0.5% to 1.7% of potassium feldspar, 0.5% to 1.0% of plagioclase, 0.4% to 0.7% of kaolinite, 0.2% to 0.5% of montmorillonite, 0.1% to 1% of pyrite, and other unmeasurable impurities and moisture.

3. The process for preparing ink according to claim 1, characterized in that: The auxiliary material is prepared by compounding bile, flavor liquid, blackening agent and stabilizer in a mass ratio of 3-8:5-10:10-15:1-3.

4. The process for preparing ink according to claim 3, characterized in that: The bile is prepared by compounding pig bile, chicken bile, bear bile and snake bile in a volume ratio of 1:1:0.01 to 0.1:0.

5.

5. The process for preparing ink according to claim 3, characterized in that: The spice liquid is prepared by mixing cloves, cinnamon bark, ash bark, sandalwood and gamboge in a mass ratio of 5-6:4-5:3-4:3-4:1-2, and then crushing, boiling and filtering.

6. The process for preparing ink according to claim 1, characterized in that: The raw materials of the gelatin are buffalo hide, yellow cow hide, ox horn, fish skin and donkey hide, which are mixed in a mass ratio of 20:20:3-4:5-10:2-4 and then boiled.

7. The process for preparing ink according to claim 1, characterized in that: The usage ratio of the matured graphite powder, gelatin, auxiliary materials, water, oil, borneol and artificial musk is 350g:110-120g:70-80g:350-400mL:2g:2g:0.8-1.0g.

8. An ink, characterized in that: The invention is prepared by the preparation process described in any one of claims 1 to 7.