White carbon black production device taking fluorine-containing silicon slag as raw material

By using a high-shear reactor and a mother liquor recycling technology, the problems of resource waste and environmental pollution in traditional silica production have been solved, enabling efficient and low-cost production of high-purity silica and improving production efficiency and product quality.

CN223542954UActive Publication Date: 2025-11-14湖北宜化氟化工有限公司
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Patent Information

Application Number
CN202422073114.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-08-26
Publication Date
2025-11-14
Estimated Expiration
2034-08-26

AI Technical Summary

Technical Problem

Traditional methods of producing silica involve resource waste, high energy consumption, and environmental pollution. Existing methods for producing silica using fluorinated silica slag are complex, costly, and difficult to control in terms of product purity and quality.

Method used

By employing high-shear reactor technology, fluorinated silicon slag and sodium hydroxide solution are rapidly dissolved in a high-shear stirrer at 80-100℃. Combined with pH adjustment and crystallization aging in the crystallization tank, the dissolution and crystallization time is shortened. The mother liquor is recycled, thus achieving efficient and low-cost production of high specific surface area Class A silica.

Benefits of technology

It significantly improved production efficiency, shortened the dissolution time and crystallization aging time of silicon slag, increased product purity and specific surface area, reduced waste liquid discharge, and achieved efficient resource utilization and environmental protection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model provides a white carbon black production device taking fluorine-containing silicon slag as a raw material, which is characterized in that a sodium hydroxide solution tank and a silicon slag slurry tank are communicated with a dissolving tank, the dissolving tank is communicated with a crystal transformation tank, high-shear reactors are arranged in the dissolving tank and the crystal transformation tank, the crystal transformation tank is communicated with a crystallization tank, and the crystallization tank is communicated with a washing device through a filter. The washing device is communicated with the drying system. The application of the high-shear reactor obviously shortens the dissolving time of the silicon slag and improves the production efficiency. By using the crystal modifier and the crystallization regulator, the crystallization process of the white carbon black is optimized, and the purity and the specific surface area of the product are improved. And the crystallization and aging time is shortened to 20-40 minutes from the traditional 2-6 hours, so that the production efficiency is remarkably improved. And the recycling of the dissolved mother liquor improves the resource utilization rate, reduces the discharge of waste liquid and realizes environment-friendly production.
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Description

Technical Field

[0001] This utility model relates to the field of silica production, and in particular to a silica production apparatus using fluorinated silica slag as raw material. Background Technology

[0002] In the chemical industry, silica (also known as silica gel or silicon dioxide) has a wide range of applications. It is widely used as a reinforcing agent for rubber and plastics, a filler for paints and coatings, an abrasive in toothpaste, and as a catalyst carrier and insulating material. Traditional silica production methods mainly include precipitation and gas-phase methods. While these methods can produce high-quality silica products, they also suffer from problems such as resource waste, high energy consumption, and environmental pollution.

[0003] With industrial development, fluorosilicon slag has become an important byproduct. It mainly originates from the production processes of the fluorochemical and phosphate chemical industries, containing large amounts of silica and fluorides. If this fluorosilicon slag is not effectively treated, it will not only waste resources but also cause serious environmental pollution. Therefore, how to effectively utilize the silica component in fluorosilicon slag and turn waste into treasure has become a current research hotspot.

[0004] In the prior art, there are several methods for producing precipitated silica using fluorinated silica slag. For example, CN102938462A discloses a method for preparing precipitated silica from fluorosilicic acid waste liquid. This method involves decomposing fluorosilicic acid with sulfuric acid under acidic conditions to generate silica gel, which is then washed and dried to obtain the precipitated silica product. CN104386711A discloses a method for preparing precipitated silica from sodium fluorosilicate waste liquid. This method involves decomposing sodium fluorosilicate with lime milk at high temperature to generate silica gel, which is then filtered, washed, and dried to obtain the precipitated silica.

[0005] While these methods have achieved some degree of resource utilization of fluorinated silica slag, they still have many shortcomings. For example, the reaction process is complex and energy consumption is high, the purity and quality of the generated silica product are difficult to control, and the wastewater and waste gas generated during the process require secondary treatment, increasing treatment costs and environmental burden.

[0006] Therefore, developing a new, efficient, and environmentally friendly technology for the resource utilization of fluorinated silica slag to produce high-quality silica in a high-efficiency and low-cost manner is of significant practical importance. This not only enables the reuse of waste resources and reduces environmental pollution but also meets market demand for high-performance silica. The current challenge lies in finding an innovative technological path that simplifies the production process, improves product purity and quality, reduces energy consumption and costs, and minimizes environmental impact. Utility Model Content

[0007] The main objective of this invention is to provide a silica production apparatus that uses fluorinated silica slag as raw material, addressing the problems of traditional silica production methods, which primarily include precipitation and gas-phase methods. While these methods can produce high-quality silica, they also suffer from resource waste, high energy consumption, and environmental pollution.

[0008] To solve the above-mentioned technical problems, the technical solution adopted by this utility model is: a white carbon black production device using fluorinated silicon slag as raw material, wherein the sodium hydroxide solution tank and the silicon slag slurry tank are connected to the dissolving tank, the dissolving tank is connected to the crystallization tank, both the dissolving tank and the crystallization tank are equipped with high shear reactors, the crystallization tank is connected to the crystallization tank, the crystallization tank is connected to the washing device through the filter, and the washing device is connected to the drying system.

[0009] In the preferred embodiment, the top of the crystallization tank is connected to the crystallization tank via a mother liquor recovery pipe.

[0010] In the preferred embodiment, the crystal transfer tank is also equipped with an additive addition pipe, and the crystal transfer agent tank, crystallization regulator tank and dilute sulfuric acid tank are connected to the crystal transfer tank through the additive addition pipe.

[0011] In a preferred embodiment, the high-shear reactor includes a first drive motor connected to a rotating shaft. A shearing paddle is provided at the lower end of the rotating shaft. A support frame is also provided below the first drive motor. The lower end of the support frame extends toward the shearing paddle, and a shearing shroud is provided at the end of the support frame. The shearing paddle is located inside the shearing shroud, and the surface of the shearing shroud has multiple holes.

[0012] In the preferred embodiment, the rotating shaft is also provided with multiple rotating blades.

[0013] In the preferred embodiment, the bottom of the dissolving tank is also provided with multiple downward-sloping auxiliary shearing rods, which are positioned on the outer ring of the shearing cover.

[0014] In the preferred embodiment, a second drive motor is provided above the crystallization tank, and multiple scrapers are provided inside the crystallization tank. The scrapers are connected to the second drive motor through a rotating shaft.

[0015] In the preferred embodiment, the drying system is connected to the storage tank via a transmission belt.

[0016] In the preferred embodiment, the temperature inside the dissolving tank is 80-100℃.

[0017] This invention provides a precipitated silica production apparatus using fluorinated silica slag as raw material. The apparatus employs high-shear reactor technology, achieving a high-efficiency, low-cost continuous production process. Fluorinated silica slag and sodium hydroxide solution are added to the high-shear reactor. At a reaction temperature of 80-100 degrees Celsius, a high-shear stirrer intensifies the dissolution process, and the resulting solution is transported to a crystallization tank. In the crystallization tank, a crystallization agent, a crystallization regulator, and dilute sulfuric acid are added through an additive inlet to adjust the pH value, ensuring thorough mixing of the slurry. The mixed slurry is then transported to a crystallization tank for crystallization and aging. The application of the high-shear reactor reduces the silica slag dissolution time from the traditional 30 minutes to 2 hours to 3-5 minutes, and the crystallization and aging time is significantly reduced from 2-6 hours to 20-40 minutes. The crystallized mixture is filtered, washed, and dried to finally obtain high-specific-surface-area Class A precipitated silica. The mother liquor is recycled, achieving efficient resource utilization and environmental protection. Attached Figure Description

[0018] The present invention will be further described below with reference to the accompanying drawings and embodiments:

[0019] Figure 1 This is a layout diagram of the production system of this utility model;

[0020] Figure 2 This is a structural diagram of the high-shear reactor of this utility model;

[0021] Figure 3 This is a structural diagram of the crystallization tank of this utility model.

[0022] In the diagram: 1. Dissolving tank; 2. High shear reactor; 201. First drive motor; 202. Support frame; 203. Rotating shaft; 204. Rotating blade; 205. Shear hood; 206. Shearing paddle; 207. Auxiliary shearing rod; 3. Crystallization tank; 4. Crystallization tank; 401. Second drive motor; 402. Scraper; 5. Filter; 6. Washing device; 7. Drying system; 8. Dissolving mother liquor recovery pipeline; 9. Sodium hydroxide solution tank; 10. Silica slag slurry tank; 11. Additive addition pipe; 12. Storage tank. Detailed Implementation

[0023] Example 1

[0024] like Figures 1-3 As shown, a silica production device using fluorinated silica slag as raw material is provided. Sodium hydroxide solution tank 9 and silica slag slurry tank 10 are connected to dissolving tank 1. Dissolving tank 1 is connected to crystallization tank 3. Both dissolving tank 1 and crystallization tank 3 are equipped with high-shear reactors 2. Crystallization tank 3 is connected to crystallization tank 4. Crystallization tank 4 is connected to washing device 6 through filter 5. Washing device 6 is connected to drying system 7.

[0025] In dissolution tank 1, sodium hydroxide solution and fluorinated silicon slag slurry are added through sodium hydroxide solution tank 9 and silicon slag slurry tank 10 respectively, allowing the fluorinated silicon slag to dissolve rapidly in high-shear reactor 2. The high-shear reactor utilizes high-speed shear force, reducing the dissolution time of silicon slag from the traditional 30 minutes to 2 hours to 3-5 minutes, significantly improving production efficiency. The dissolved silicon slag solution is then transported to crystal transformation tank 3 via pipeline.

[0026] In the crystallization tank 3, crystallization agent, crystallization regulator, and dilute sulfuric acid are added through the additive addition pipe 11 to adjust the pH value to an appropriate range and mix thoroughly. The mixed slurry is then transported to the crystallization tank 4 for crystallization and aging, reducing the crystallization and aging time from the traditional 2-6 hours to 20-40 minutes. The crystallized mixture undergoes solid-liquid separation through the filtration device 5. The resulting silica crystals are washed through the washing device 6 to remove residual impurities, and then enter the drying system 7 for drying to obtain a high specific surface area Class A silica product.

[0027] In the preferred embodiment, the top of the crystallization tank 4 is connected to the crystal transfer tank 3 via a mother liquor recovery pipe 8. The mother liquor recovery pipe 8 returns the mother liquor generated in the crystallization tank 4 to the crystal transfer tank 3 for recycling, which helps to save resources and reduce wastewater discharge.

[0028] The recycling of dissolving mother liquor can be achieved by improving the recycling system or introducing new separation technologies (such as membrane separation and ion exchange), thereby increasing resource utilization, reducing waste liquid discharge, and lowering production costs and environmental impact.

[0029] In the preferred embodiment, the crystallization tank 3 is also equipped with an additive addition pipe 11. The crystallization agent tank, crystallization regulator tank, and dilute sulfuric acid tank are connected to the crystallization tank 3 via the additive addition pipe 11. In the crystallization tank 3, the crystallization agent, crystallization regulator, and dilute sulfuric acid are added through the additive addition pipe 11 to adjust the pH value to an appropriate range and mix thoroughly. The mixed slurry is then transported to the crystallization tank 4 for crystallization aging, reducing the crystallization aging time from the traditional 2-6 hours to 20-40 minutes.

[0030] In a preferred embodiment, the high-shear reactor 2 includes a first drive motor 201, which is connected to a rotating shaft 203. A shearing paddle 206 is provided at the lower end of the rotating shaft 203. A support frame 202 is also provided below the first drive motor 201. The lower end of the support frame 202 extends toward the shearing paddle 206, and a shearing cover 205 is provided at the end of the support frame 202. The shearing paddle 206 is disposed inside the shearing cover 205, and the surface of the shearing cover 205 is provided with multiple holes.

[0031] The first drive motor 201 drives the rotating shaft 203 to rotate. The rotating shaft 203 drives the shearing paddle 206 mounted at its lower end to rotate together. The support frame 202 fixes the entire structure and ensures that the shearing paddle 206 operates stably within the shearing shroud 205. Multiple holes on the shearing shroud 205 allow material to flow freely, while the shearing paddle 206 rotates inside the shearing shroud 205, generating strong shearing force and accelerating the dissolution process of the silica slag.

[0032] In a preferred embodiment, the rotating shaft 203 is further provided with multiple rotating blades 204. The rotating blades 204 provide additional stirring action, which helps to better disperse and mix the materials, further improving the dissolution efficiency.

[0033] In a preferred embodiment, the bottom of the dissolving tank 1 is further provided with multiple downward-sloping auxiliary shearing rods 207, which are positioned on the outer ring of the shear shield 205. These downward-sloping auxiliary shearing rods, positioned on the outer ring of the shear shield 205, work in conjunction with the shearing paddle 206 to achieve a better mixing effect. The combined use of the auxiliary shearing rods 207 and the shearing paddle 206 helps to better disperse and mix the materials, further improving the dissolving efficiency.

[0034] In a preferred embodiment, a second drive motor 401 is installed above the crystallization tank 4, and multiple scrapers 402 are installed inside the crystallization tank 4. The scrapers 402 are connected to the second drive motor 401 via a rotating shaft. The second drive motor 401 drives the rotating shaft to rotate. The rotating shaft drives the multiple scrapers 402 to rotate, stirring the slurry in the crystallization tank 4. The stirring by the scrapers 402 helps to improve the material distribution during the crystallization process, making the crystallization more uniform and the crystallization effect better.

[0035] In the preferred embodiment, the drying system 7 is connected to the storage tank 12 via a transmission belt. The storage tank 12 is used to store the silica product.

[0036] In the preferred embodiment, the temperature inside the dissolution tank 1 is 80-100℃. Maintaining the temperature inside the dissolution tank 1 between 80-100℃ accelerates the dissolution process of fluorinated silicon slag in the sodium hydroxide solution. Within this temperature range, the high-shear reactor 2 can operate more efficiently, reducing the dissolution time of the silicon slag from the traditional 30 minutes to 2 hours to 3-5 minutes, significantly improving production efficiency.

[0037] Utilizing the efficient mixing and shear force of the high-shear reactor 2, the dissolution time of fluorinated silica slag in sodium hydroxide solution is significantly shortened to 3-5 minutes. The dissolved silica slag solution is then subjected to pH adjustment in the crystallization tank 3 by adding a crystallization agent, a crystallization regulator, and dilute sulfuric acid to ensure thorough mixing. The slurry is then transferred to the crystallization tank for crystallization and aging, reducing the time from 2-6 hours to 20-40 minutes. Finally, after solid-liquid separation, washing, and drying, high-purity, high-specific-surface-area Class A silica product is obtained. Simultaneously, the recycling of the mother liquor improves resource utilization efficiency, reduces wastewater discharge, and achieves green production.

[0038] Solvent alternatives: In addition to using sodium hydroxide solution, other alkaline solutions such as potassium hydroxide solution or sodium carbonate solution can be tried to dissolve fluorinated silicon slag in order to optimize reaction conditions and production costs.

[0039] Alternative acidity regulators: In addition to dilute sulfuric acid, other acidic solutions such as hydrochloric acid or phosphoric acid can be used to adjust the pH value in the crystallization tank, thereby optimizing the crystallization conditions and efficiency of silica.

[0040] Resource recycling and substitution: The recycling and reuse of dissolving mother liquor can be achieved by improving the recycling system or introducing new separation technologies (such as membrane separation, ion exchange, etc.), thereby improving resource utilization, reducing waste liquid discharge, and lowering production costs and environmental impact.

[0041] The above embodiments are merely preferred technical solutions of this utility model and should not be considered as limitations on this utility model. The protection scope of this utility model should be the technical solution described in the claims, including equivalent substitutions of the technical features described in the claims. That is, equivalent substitutions and improvements within this scope are also within the protection scope of this utility model.

Claims

1. A precipitated silica production apparatus using fluorinated silica slag as raw material, characterized in that: sodium hydroxide... The solution tank (9) and the silicon slag slurry tank (10) are connected to the dissolving tank (1), the dissolving tank (1) is connected to the crystallization tank (3), the dissolving tank (1) and the crystallization tank (3) are both equipped with high shear reactors (2), the crystallization tank (3) is connected to the crystallization tank (4), the crystallization tank (4) is connected to the washing device (6) through the filter (5), and the washing device (6) is connected to the drying system (7); The high shear reactor (2) includes a first drive motor (201), which is connected to a rotating shaft (203). The lower end of the rotating shaft (203) is provided with a shear blade (206). A support frame (202) is also provided below the first drive motor (201). The lower end of the support frame (202) extends toward the shear blade (206), and a shear shield (205) is provided at the end of the support frame (202). The shear blade (206) is located inside the shear shield (205), and the surface of the shear shield (205) is provided with multiple holes. The bottom of the melting tank (1) is also provided with multiple downward-sloping auxiliary shearing rods (207), which are located on the outer ring of the shearing cover (205).

2. The silica production apparatus using fluorinated silica slag as raw material according to claim 1, characterized in that: The top of the crystallization tank (4) is connected to the crystallization tank (3) through the mother liquor recovery pipe (8).

3. The silica production apparatus using fluorinated silica slag as raw material according to claim 1, characterized in that: The crystal transfer tank (3) is also equipped with an additive addition pipe (11). The crystal transfer agent tank, the crystallization regulator tank and the dilute sulfuric acid tank are connected to the crystal transfer tank (3) through the additive addition pipe (11).

4. The silica production apparatus using fluorinated silica slag as raw material according to claim 2, characterized in that: The rotating shaft (203) is also equipped with multiple rotating blades (204).

5. The silica production apparatus using fluorinated silica slag as raw material according to claim 1, characterized in that: A second drive motor (401) is provided above the crystallization tank (4), and multiple scrapers (402) are provided inside the crystallization tank (4). The scrapers (402) are connected to the second drive motor (401) through a rotating shaft.

6. The silica production apparatus using fluorinated silica slag as raw material according to claim 1, characterized in that: The drying system (7) is connected to the storage box (12) via a drive belt.

7. The silica production apparatus using fluorinated silica slag as raw material according to claim 1, characterized in that: The temperature inside the dissolving tank (1) is 80-100℃.

Citation Information

Patent Citations

  • Composite lithium-ion doping battery positive pole material and preparation method thereof

    CN102938462A

  • Method for preparing sodium fluoride from defluorination residue generated in production of phosphoric acid by wet process

    CN104386711A