EZHOU ANJEKA TECHNOLOGY CO.,Ltd Anjeka@anjeka.net 86-0711-5117111
Anjeka Experimental Report
Study on the storage stability of ceramic ink
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Experimental project: Study on the storage stability of ceramic ink
Experimental category: Dispersant, anti settling agent testing
Experimenter: Product Application Engineer Xinzhong Zhai
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Abstract:Ceramic inks were prepared using Anjikang dispersants 6042A and 6042B, anti-settling agents 4311, 4360, 6701, 972, and bentonite. The stability of the ceramic inks was evaluated by measuring the particle size, viscosity, centrifugal sedimentation rate, and sedimentation rate after thermal storage, as well as the hard settling rate. The experimental results indicate that the white oil-based ceramic ink prepared with Anjeka 6042B dispersant exhibits the best storage stability.
Keywords: dispersant, anti settling agent, particle size, viscosity, centrifugal precipitation rate1.
1.Objective
Ceramic inks were prepared using different formulations incorporating Anjeka dispersants 6042A and 6042B, anti-settling agents 4311, 4360, 6701, 972, and bentonite. The stability of the ceramic inks prepared with different formulations was investigated by evaluating particle size, viscosity, centrifugal sedimentation rate, as well as sedimentation rate and hard settling rate after thermal storage.
Reagents:
Ceramic colorant (encapsulated red, Guose), dispersants Anjeka 6042A and Anjeka 6042B, anti-settling agents Anjeka 4311, Anjeka 4360, Anjeka 6701, 972, bentonite, white oil, cocoate, isopropyl laurate, ceramic pigment, and Mirui ceramic ink sample.
Instruments:
Centrifuge (Model 80-2B, Jiangsu Jinyi Instrument Technology Co., Ltd.), nanoparticle size analyzer (Model BeNano 90, Dandong Bettersize Instruments Co., Ltd.), oscillating disperser, rotational digital viscometer, ultrasonic disperser, oven.
White oil No. 10, cocoate, and dispersant were mixed in a certain proportion until homogeneous. The ceramic colorant was then added and mixed thoroughly. Zirconia beads (0.3 mm diameter) in an amount three times the mass of the slurry were added, and the mixture was placed in an oscillating disperser for dispersion.
The inks were stored in an oven at 50°C for 72 hours.
Particle Size Measurement of Ceramic Colorant in Ink:
The ground slurry was diluted 10,000 times with white oil. The particle size of the colorant in the diluted ink was measured using a nanoparticle size analyzer.
Centrifugal Sedimentation Rate:
The inks were centrifuged at 3000 rpm for either 5 minutes or 10 minutes as specified.
Viscosity:
The viscosity of the inks was measured at 15°C using a rotational viscometer.
Table 1. Experimental Formulations for Different Dispersants and Dosages
| Raw Material | 1# | 2# | 3# | 4# | 5# | 6# | Supplier |
| White Oil | 42.5 | 43.35 | 44.2 | 42.5 | 43.35 | 44.2 | Guose |
| Cocoate | 7.5 | 7.65 | 7.8 | 7.5 | 7.65 | 7.8 | Mirui |
| Dispersant 6042A | 5 | 4 | 3 | Anjeka | |||
| Dispersant 6042B | 5 | 4 | 3 | Anjeka | |||
| Encapsulated Red | 45 | 45 | 45 | 45 | 45 | 45 | Guose |
After 8 hours of oscillating grinding, the particle size, viscosity, and centrifugal sedimentation rate were measured. The results are shown in Table 3.
Table 3. Particle Size, Viscosity, and Centrifugal Sedimentation Rate
| 1# | 2# | 3# | 4# | 5# | 6# | |
| Z-Average Particle Size(nm) | 225.54 | 369.99 | 275.08 | 295.26 | 273.09 | 292.15 |
| Viscosity(mpa.s) | 291.9 | 551. 1 | 4340 | 52.64 | 421. 1 | 6076 |
| Centrifugal Sedimentation Rate%(5min) | 13. 12 | 13.48 | 21.30 | 5.36 | 12.39 | 21.36 |
| Centrifugal Sedimentation Rate%(10min) | 17. 11 | 24.18 | 32.44 | 7.69 | 17.29 | 26.28 |
At a dispersant dosage of 5%, dispersant 6042A demonstrates superior particle size reduction compared to dispersant 6042B; however, its wetting and viscosity reduction performance, as well as its centrifugal sedimentation rate, are inferior to those of dispersant 6042B.
Table 4. Experimental Formulations with Different Solvents
| Raw Material | 1# | 2# | 3# | Supplier |
| White Oil | 50 | 42.5 | 42.5 | Guose |
| Cocoate | 7.5 | Mirui | ||
| Isopropyl Laurate | 7.5 | |||
| 6042B | 5 | 5 | 5 | Anjeka |
| Encapsulated Red | 45 | 45 | 45 | Guose |
Table 5. Particle Size, Viscosity, and Centrifugal Sedimentation Rate
| 1# | 2# | 3# | |
| Z-Average Particle Size(nm) | 242.78 | 295.26 | 309.5 |
| Viscosity(mpa.s) | 65 | 52.64 | 60 |
| Centrifugal Sedimentation Rate (%) (5 min) | 1.9 | 5.36 | 6.75 |
From the above results, it can be observed that different solvents have a significant impact on the centrifugal sedimentation rate. Among the formulations, pure white oil (Sample 1#) exhibits the best performance, while isopropyl laurate (Sample 3#) shows the worst performance.
Based on the experimental results in Section 3.1, dispersant 6042B was selected at a dosage of 5%, and the grinding time was varied to 3, 4, and 5 hours. The experimental formulations are shown in Table 6.
Table 6. Ceramic Ink Formulations
| Grinding 3h | Grinding4h | Grinding5h | Supplier | |
| Mixed Oil (White Oil : Cocoate = 85:15) | 50 | 50 | 50 | Mirui |
| 6042B | 5 | 5 | 5 | Anjeka |
| Ceramic Pigment | 45 | 45 | 45 | Mirui |
The particle size, viscosity, and centrifugal sedimentation rate after grinding are shown in Table 7.
Table 7. Particle Size, Viscosity, and Centrifugal Sedimentation Rate
| Grinding3h | Grinding4h | Grinding5h | Mirui Sample | |
| Z-Average Particle Size(nm) | 416.16 | 389. 12 | 306.05 | 324.15 |
| D50(nm) | 443.01 | 433.72 | 309.25 | 355.08 |
| D90(nm) | 8471.96 | 950.22 | 588.35 | 536.82 |
| Viscosity(mpa.s) | 32.6 | 39.3 | 46.1 | 43.07 |
| Centrifugal Sedimentation Rate (%) (10min) | 26.03 | 10.84 | 7.73 | 7.28 |
Table 8. Experimental Formulations
| 1# | 2# | 3# | 4# | 5# | 6# | Supplier | |
| Mixed Oil (White Oil : Cocoate = 85:15) | 50 | 49 | 49.7 | 49.7 | 49.7 | 49.7 | Mirui |
| Dispersant 6042B | 5 | 5 | 5 | 5 | 5 | 5 | Anjeka |
| Ceramic Pigment | 45 | 45 | 45 | 45 | 45 | 45 | Mirui |
| Anti-Settling Agent 4311 | 1 | Anjeka | |||||
| Anti-Settling Agent 4360 | 1 | Anjeka | |||||
| Anti-Settling Agent 6701 | 0.3 | Anjeka | |||||
| Anti-Settling Agent 972 | 0.3 | Anjeka | |||||
| Bentonite | 0.3 | Fenghong |
Table 9. Particle Size and Centrifugal Sedimentation Rate
| 1# | 2# | 3# | 4# | 5# | 6# | |
| Z-Average Particle Size After 3h Grinding(nm) | 416.16 | 321.58 | 465.26 | 334.77 | 673.63 | 435.38 |
| Z-Average Particle Size After 5h Grinding(nm) | 306.05 | 315.21 | 338.45 | 262.22 | 283.33 | 453 |
| Centrifugal Sedimentation Rate after 3h Grinding(%) (10 min) | 26.03 | 24.88 | 45.23 | 18.70 | 23.19 | 23.93 |
|
Centrifugal Sedimentation Rate after 5h Grinding(%) (10 min)
|
7.73 | 20.40 | 42. 12 | 17.46 | 11.69 | 25.49 |
After 3 hours of grinding, when the particle size of the slurries had not yet reached the required specification, all formulations except 3# exhibited anti-settling effects, with Sample 4# showing the best performance.
3.5 Effect of Different Anti-Settling Agents on the Thermal Storage Stability of Ceramic Inks
Ceramic inks were prepared according to the formulations in Table 10 and ground for 5 hours. The thermal storage stability was evaluated after storage in an oven at 50°C for 72 hours. The results are shown in Table 11.
The sedimentation rate and hard settling rate were calculated as follows:
Sedimentation Rate = (Initial ink height − Height of the lower layer after stratification) / Initial ink height × 100%
Hard Settling Rate = Mass of hard sediment / Total mass of ink × 100%
Table 10. Experimental Formulations
| 1# | 2# | 3# | 4# | 5# | Supplier | |
| Mixed Oil (White Oil : Cocoate = 85:15) | 49 | 50 | 48.7 | 48.7 | 48.7 | Mirui |
| Dispersant 6042B | 6 | 5 | 6 | 6 | 6 | Anjeka |
| Ceramic Pigment | 45 | 45 | 45 | 45 | 45 | Mirui |
| Anti-Settling Agent 972 | 0.3 | Anjeka | ||||
| Anti-Settling Agent 6701 | 0.3 | Anjeka | ||||
| Bentonite | 0.3 | Fenghong |
Table 11. Thermal Storage Stability Results
| 1# | 2# | 3# | 4# | 5# | Mirui Sample | |
| Z-Average Particle Size(nm) | 305.05 | 337.5 | 282.6 | 272.22 | 443 | 324.15 |
| Z-Average Particle Size(%) | 0 | 7.8 | 8.3 | 10.2 | 53.3 | 9.5 |
| Hard Settling Rate (%) | 1.3 | 5.3 | 2.0 | 2.5 | 5.8 | 4.3 |
From the above table and chart, the following observations can be made:
For the anti-settling agents tested in this experiment, the results indicate that they do not provide anti-settling effects under thermal storage conditions.
Increasing the dosage of dispersant 6042B improves thermal storage stability. When the dosage is increased to 6%, the performance is superior to that of the reference sample.
Dispersant Anjeka 6042A exhibits slightly better particle size reduction performance than Anjeka 6042B, but its wetting, viscosity reduction, and stability performance are inferior to those of Anjeka 6042B.
The dosage of dispersant has a significant impact on particle size and viscosity. Within a certain dosage range, increasing the dispersant content reduces particle size and viscosity while improving stability.
The choice of solvent has a considerable effect on stability, with pure white oil yielding the best performance.
When particle size and viscosity are reduced to a certain range, viscosity has a minor effect on stability, while larger Z-average particle size and D90 particle size lead to poorer stability.
For the anti-settling agents tested in this experiment, once the slurry particle size reaches the required specification for the product, the anti-settling agents lose their stabilizing effect.
Increasing the dosage of dispersant 6042B improves thermal storage stability, and at a dosage of 6%, the performance is superior to that of the reference sample.