A method for improving the dispersibility of a laboratory titanium dioxide sand mill system

By employing steps such as ultrasonic dispersion, pH adjustment, and vertical sand milling, the problem of poor dispersibility of titanium dioxide in the laboratory was solved, resulting in better dispersion and product quality.

CN117327410BActive Publication Date: 2026-06-12PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
Filing Date
2023-09-27
Publication Date
2026-06-12

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Abstract

The application discloses a method for improving dispersibility of a laboratory titanium dioxide sand grinding system, and comprises the following steps: preparing titanium dioxide slurry by using titanium dioxide and deionized water, dispersing the titanium dioxide slurry in an ultrasonic cell disrupter, fully reacting in an ultrasonic environment after adding isopropanol amine, adjusting pH in the ultrasonic environment, adding sodium silicate stock solution, uniformly stirring and dispersing the slurry in a stirrer, then adding zirconium beads with the same mass as the titanium dioxide, finally, placing the slurry in a vertical sand mill for sand grinding, sieving by using a vibrating screen after the sand grinding is completed, and obtaining target slurry; the application provides a laboratory rutile titanium dioxide sand grinding treatment method which is convenient to operate and has excellent dispersing effect, realizes effective dispersion of titanium dioxide roller grinding primary products, makes titanium dioxide particles after sand grinding in a more uniform and stable state, significantly improves process efficiency of post-treatment, improves product quality of the titanium dioxide, and achieves the purpose of effectively guiding improvement of a factory titanium dioxide production process.
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Description

Technical Field

[0001] This invention specifically relates to the field of titanium dioxide technology, and more specifically to a method for improving the dispersibility of a laboratory titanium dioxide sand milling system. Background Technology

[0002] Titanium dioxide is currently the most widely used and effective white pigment, widely applied in coatings, plastics, inks, rubber, and other fields. However, during the production process, due to the photochemical activity and extremely high surface energy of TiO2, surface treatment is necessary to improve its dispersibility and surface activity, and enhance the product's weather resistance, anti-chalking properties, and other application performance. To obtain a uniform hydrated oxide surface film, the titanium dioxide particles must be completely dispersed before inorganic coating; otherwise, the uniformity and light scattering of the surface coating layer will be directly affected, thereby reducing the pigment's optical properties and overall performance.

[0003] Laboratory titanium dioxide sand milling process can provide indispensable guidance for improving the quality of titanium dioxide in industrial settings and is the cornerstone of titanium dioxide quality improvement. The factors affecting the dispersibility of the laboratory sand milling system mainly include three categories: dispersed phase, dispersion medium, and applied mechanical force. Among them, the dispersant added during the grinding process determines the dispersed phase and dispersion medium, greatly affects the slurry dispersion effect, has a significant impact on the viscosity of the system, and can improve the sand milling efficiency.

[0004] The existing laboratory titanium dioxide has low dispersibility, high viscosity, and poor dispersion effect, which affects the subsequent processing of titanium dioxide and results in poor product quality. Summary of the Invention

[0005] The purpose of this invention is to provide a method for improving the dispersibility of laboratory titanium dioxide sand milling systems, in order to solve the problems mentioned in the background art where the laboratory titanium dioxide has low dispersibility, high viscosity, and poor dispersion effect, which affects the subsequent processing of titanium dioxide and leads to poor product quality.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A method for improving the dispersibility of a laboratory titanium dioxide sand milling system includes the following steps:

[0008] Step 1: Prepare titanium dioxide slurry, which includes titanium dioxide and deionized water;

[0009] Step 2: Disperse the titanium dioxide slurry in an ultrasonic cell disruptor, add isopropanolamine after 20 minutes, and allow it to react fully in an ultrasonic environment.

[0010] Step 3: Adjust the pH under ultrasonic conditions and add sodium silicate stock solution;

[0011] Step 4: Pour the slurry into a mixer and stir evenly to disperse it;

[0012] Step 5: Take out the slurry and add zirconium beads of equal mass to the titanium dioxide. The zirconium beads should have a particle size of 0.6-0.8 mm. Then place the slurry in a vertical sand mill for sand milling.

[0013] Step 6: After sand milling, use a vibrating screen to sieve the material to obtain the target slurry.

[0014] As a further aspect of the present invention: in step one, the concentration of the titanium dioxide slurry is 400-500 g / L.

[0015] As a further aspect of the present invention: In step one, the method for preparing titanium dioxide slurry is as follows: Select a rutile titanium dioxide initial product after roller milling, add deionized water and slurry until the slurry concentration is 400-500g / L.

[0016] As a further aspect of the present invention: in step two, the duration of the reaction in the ultrasonic environment is 20-50 minutes.

[0017] As a further aspect of the present invention: in step two, the water temperature in the ultrasonic cell disruptor is 30°C and the frequency is 100-150Hz.

[0018] As a further aspect of the present invention: in step two, the mass fraction of isopropanolamine is 0.05-0.2% of the mass of titanium dioxide.

[0019] As a further aspect of the present invention: in step three, the pH value is adjusted within the range of 10.5-11.2.

[0020] As a further aspect of the present invention: in step three, the mass fraction of sodium silicate is 0.1-0.3% of the mass of titanium dioxide.

[0021] As a further embodiment of the present invention: in step four, the stirring speed is 300-500 r / min, and the stirring time is 20-30 min.

[0022] As a further aspect of the present invention: in step five, the grinding speed of the vertical sand mill is 3000 r / min, and the grinding time is 30 min.

[0023] Compared with existing technologies, the beneficial effects of this invention are as follows: This invention utilizes titanium dioxide and deionized water to prepare a titanium dioxide slurry. The titanium dioxide slurry is dispersed in an ultrasonic cell disruptor, and isopropanolamine is added for full reaction in an ultrasonic environment. The pH is adjusted under ultrasonic conditions, and sodium silicate stock solution is added. The slurry is then poured into a stirrer for uniform stirring and dispersion. Then, zirconium beads of equal mass to titanium dioxide are added. Finally, the slurry is placed in a vertical sand mill for sand milling. After sand milling, it is sieved using a vibrating screen to obtain the target slurry. This provides a convenient and highly effective laboratory sand milling method for rutile titanium dioxide, achieving effective dispersion of the initial product from the roller milling of titanium dioxide. This results in a more uniform and stable state for the sand-milled titanium dioxide particles, significantly improving the efficiency of post-processing, enhancing the quality of titanium dioxide products, and effectively guiding improvements in factory titanium dioxide production processes. Attached Figure Description

[0024] Figure 1 A flowchart of a method for improving the dispersibility of a laboratory titanium dioxide sand milling system. Detailed Implementation

[0025] The present application will now be further described in conjunction with the accompanying drawings and specific embodiments. It should be noted that, without conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0026] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be further described in detail below with reference to specific examples and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative and are not intended to limit the scope of this application.

[0027] It should be noted that all uses of "first" and "second" in the embodiments of the present invention are for the purpose of distinguishing two different entities or different parameters with the same name. Therefore, "first" and "second" are merely for convenience of expression and should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion, such as other steps or units inherent in a process, method, system, product, or device that includes a series of steps or units.

[0028] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0029] The flowchart shown in the attached diagram is for illustrative purposes only and does not necessarily include all content and operations / steps, nor does it necessarily have to be performed in the order described. For example, some operations / steps can be broken down, combined, or partially merged, so the actual execution order may change depending on the actual situation.

[0030] The following detailed description of some embodiments of this application is provided in conjunction with the accompanying drawings. Unless otherwise specified, the following embodiments and features can be combined with each other.

[0031] Laboratory titanium dioxide sand milling process can provide indispensable guidance for improving the quality of titanium dioxide in industrial settings and is the cornerstone of titanium dioxide quality improvement. The factors affecting the dispersibility of the laboratory sand milling system mainly include three categories: dispersed phase, dispersion medium, and applied mechanical force. Among them, the dispersant added during the grinding process determines the dispersed phase and dispersion medium, greatly affects the slurry dispersion effect, has a significant impact on the viscosity of the system, and can improve the sand milling efficiency.

[0032] The existing laboratory titanium dioxide has low dispersibility, high viscosity, and poor dispersion effect, which affects the subsequent processing of titanium dioxide and results in poor product quality.

[0033] Based on this, please refer to Figure 1 In this embodiment of the invention, a method for improving the dispersibility of a laboratory titanium dioxide sand milling system includes the following steps:

[0034] Step 1: Prepare titanium dioxide slurry. The titanium dioxide slurry includes titanium dioxide and deionized water. The concentration of the titanium dioxide slurry is 400-500 g / L. In Step 1, the method for preparing the titanium dioxide slurry is as follows: Select a rutile titanium dioxide initial product after roller milling, add deionized water and slurry until the slurry concentration is 400-500 g / L.

[0035] Step 2: Disperse the titanium dioxide slurry in an ultrasonic cell disruptor. After 20 minutes, add isopropanolamine and react fully in an ultrasonic environment for 20-50 minutes. In Step 2, the water temperature in the ultrasonic cell disruptor is 30℃, the frequency is 100-150Hz, and the mass fraction of isopropanolamine is 0.05-0.2% of the mass of titanium dioxide.

[0036] Step 3: Adjust the pH to 10.5-11.2 under ultrasonic conditions, add sodium silicate stock solution. In step 3, the mass fraction of sodium silicate is 0.1-0.3% of the mass of titanium dioxide. The ultrasonic environmental conditions are the same as in step 2.

[0037] Step 4: Pour the slurry into a mixer and stir evenly to disperse it. The mixer speed is 300-500 r / min, and the stirring time is 20-30 min.

[0038] Step 5: Take out the slurry and add zirconium beads of equal mass to the titanium dioxide. The zirconium beads have a particle size of 0.6-0.8 mm. Then place the slurry in a vertical sand mill for sand milling at a speed of 3000 r / min for 30 min.

[0039] Step 6: After the sand milling is completed, use a vibrating screen to sieve the material to obtain the target slurry. The vibrating screen has a mesh size of 350.

[0040] Example 1

[0041] A primary product of rutile titanium dioxide after roller milling was selected and mixed with an appropriate amount of deionized water to form a pulp with a pulping concentration of 400 g / L. The pulp was then placed in an ultrasonic cell disruptor with a water temperature of 30℃ and a frequency of 150 Hz for 20 minutes. After that, isopropanolamine was added at a mass of 0.15% of the titanium dioxide mass, and the mixture was subjected to ultrasonic reaction for another 20 minutes. The pH of the pulp was then adjusted to 10.8 under ultrasonic conditions. Finally, sodium silicate stock solution was added at a mass of 0.3% of the titanium dioxide mass, and the mixture was stirred. The slurry was stirred and dispersed uniformly for 20 minutes at a speed of 450 r / min. The slurry was then removed, and zirconium beads with a particle size of 0.6-0.8 mm with an equal mass to titanium dioxide were added to the slurry. The slurry was then placed in a vertical sand mill for sand milling at a speed of 3000 r / min for 30 minutes. After sand milling, the slurry was sieved through a 350-mesh vibrating screen to obtain the target slurry. The particle size, viscosity, and sedimentation ratio of the target slurry were measured, and the measurement results are shown in Table 1.

[0042] Table 1

[0043]

[0044] Example 2

[0045] A primary product of rutile titanium dioxide after roller milling was selected and mixed with an appropriate amount of deionized water to form a pulp with a pulping concentration of 450 g / L. The pulp was then placed in an ultrasonic cell disruptor with a water temperature of 30℃ and a frequency of 150 Hz for 20 minutes. After that, isopropanolamine was added at a mass of 0.15% of the titanium dioxide mass, and the mixture was subjected to ultrasonic reaction for another 20 minutes. The pH of the pulp was then adjusted to 10.8 under ultrasonic conditions. Finally, sodium silicate stock solution was added at a mass of 0.3% of the titanium dioxide mass, and the mixture was stirred. The slurry was stirred and dispersed at a speed of 450 r / min for 20 min. The slurry was then removed, and zirconium beads with a particle size of 0.6-0.8 mm, equal in mass to the titanium dioxide, were added. The slurry was then placed in a vertical sand mill for grinding at a speed of 3000 r / min for 30 min. After grinding, the slurry was sieved through a 350-mesh vibrating screen to obtain the target slurry. The particle size, viscosity, and settling ratio of the target slurry were measured, and the results are shown in Table 2.

[0046] Table 2

[0047]

[0048] Example 3

[0049] A primary product of rutile titanium dioxide after roller milling was selected and mixed with an appropriate amount of deionized water to form a slurry with a concentration of 500 g / L. The slurry was then placed in an ultrasonic cell disruptor at a water temperature of 30°C and a frequency of 150 Hz for 20 minutes. After 20 minutes, isopropanolamine (0.15% of the titanium dioxide mass) was added, and the mixture was subjected to ultrasonic reaction for another 20 minutes. The pH of the slurry was then adjusted to 10.8 under ultrasonic conditions. Sodium silicate stock solution (0.3% of the titanium dioxide mass) was then added, and the mixture was stirred. The slurry was stirred and dispersed at a speed of 450 r / min for 20 min. The slurry was then removed, and zirconium beads with a particle size of 0.6-0.8 mm with an equal mass to titanium dioxide were added to the slurry. The slurry was then placed in a vertical sand mill for sand milling at a speed of 3000 r / min for 30 min. After sand milling, the slurry was sieved through a 350 mesh vibrating screen to obtain the target slurry. The particle size, viscosity, and sedimentation ratio of the target slurry were measured, and the measurement results are shown in Table 3.

[0050] Table 3

[0051]

[0052] In summary, this invention utilizes titanium dioxide and deionized water to prepare a titanium dioxide slurry. The slurry is dispersed in an ultrasonic cell disruptor, and isopropanolamine is added followed by a thorough reaction in an ultrasonic environment. The pH is adjusted under ultrasonic conditions, and sodium silicate stock solution is added. The slurry is then poured into a stirrer and uniformly dispersed. Zirconium beads of equal mass to the titanium dioxide are added, and the slurry is finally milled in a vertical sand mill. After milling, the slurry is sieved using a vibrating screen to obtain the target slurry. This provides a convenient and highly effective laboratory method for milling rutile titanium dioxide, achieving effective dispersion of the initial product from roller milling. This results in a more uniform and stable state of the milled titanium dioxide particles, significantly improving post-processing efficiency and enhancing the quality of the titanium dioxide product. Ultimately, this method effectively guides improvements in factory titanium dioxide production processes.

[0053] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0054] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for improving the dispersibility of a laboratory titanium dioxide sand milling system, characterized in that, Includes the following steps: Step 1: Prepare titanium dioxide slurry, which includes titanium dioxide and deionized water. The titanium dioxide is the initial product of rutile titanium dioxide after roller milling. Step 2: Disperse the titanium dioxide slurry in an ultrasonic cell disruptor, add isopropanolamine, and react fully in an ultrasonic environment. The water temperature in the ultrasonic cell disruptor is 30℃ and the frequency is 100-150Hz. Step 3: Adjust the pH under ultrasonic conditions and add sodium silicate stock solution. The ultrasonic conditions are the same as in Step 2. Step 4: Pour the slurry into a mixer and stir evenly to disperse it. The mixer speed is 300-500 r / min, and the stirring time is 20-30 min. Step 5: Take out the slurry, add zirconium beads of the same mass as titanium dioxide to the slurry, and then place the slurry in a vertical sand mill for sand milling. The zirconium bead particle size is 0.6-0.8mm, the sand milling speed is 3000r / min, and the sand milling time is 30min. Step 6: After sand milling, use a vibrating screen to sieve the material to obtain the target slurry.

2. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 1, characterized in that, In step one, the concentration of the titanium dioxide slurry is 400-500 g / L.

3. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 2, characterized in that, In step one, the method for preparing titanium dioxide slurry is as follows: select a rutile titanium dioxide raw material after roller milling, add deionized water and slurry until the slurry concentration is 400-500g / L.

4. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 1, characterized in that, In step two, the duration of the reaction in the ultrasonic environment is 20-50 minutes.

5. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 1, characterized in that, In step two, the mass fraction of isopropanolamine is 0.05-0.2% of the mass of titanium dioxide.

6. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 1, characterized in that, In step three, the pH value is adjusted within the range of 10.5-11.

2.

7. The method for improving the dispersibility of a laboratory titanium dioxide sand milling system according to claim 6, characterized in that, In step three, the mass fraction of sodium silicate is 0.1-0.3% of the mass of titanium dioxide.