Cooling crystallization equipment for potassium fluotantalate

Abstract

The utility model discloses equipment for cooling and crystallizing potassium fluotantalate, which comprises a cooling tank and a plurality of pipelines arranged in the cooling tank, the diameter range of the pipelines is phi 30-80mm, the bottoms of the pipelines are closed, the number of the pipelines is 8-30, the pipelines are uniformly distributed in a main pipeline with the diameter of 1000mm, and the diameter of the main pipeline is 1000 mm. The device is used for forming potassium fluotantalate crystals on the surface of a pipeline after a potassium fluotantalate solution is injected into the cooling tank, and separating the potassium fluotantalate crystals from the cooling tank or the pipeline by knocking the pipeline. According to the utility model, the cooling and crystallization speed of potassium fluotantalate is obviously improved, and the problem of slow cooling in the traditional method is solved; the contact area of the potassium fluotantalate crystal in the crystallization process is effectively increased, and the uniformity of the crystal is remarkably improved; and a solid foundation is laid for improving the overall quality of a potassium fluotantalate product, and revolutionary improvement is expected to be caused in the tantalum-niobium metallurgy field.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical equipment, in particular to cooling crystallization equipment for potassium fluorotantalate. Background Art

[0002] Potassium fluorotantalate, as a core raw material in the field of tantalum-niobium metallurgy, plays a vital role, especially in the production of high-quality metallurgical-grade and capacitor-grade tantalum powder. The preparation process of this substance involves preheating fluorotantalate to a specific temperature, followed by the addition of a mixed solution of potassium chloride and hydrofluoric acid to carry out a chemical reaction. The hot solution obtained after the reaction needs to be transferred to a cooling tank made of polyethylene (PE) or polypropylene (PP) to start the cooling process. The cooling method is flexible and diverse, and can rely on the heat dissipation of the natural environment or adopt a more active external forced cooling strategy. However, it usually takes more than 20 hours to reduce the solution temperature from 90 degrees Celsius, which is close to the boiling point, to about 30 degrees Celsius to form the final potassium fluorotantalate crystals.

[0003] A significant weakness of this cooling crystallization method is that the space in which the crystals grow is severely limited, resulting in stacking and overlapping of the crystals. This, in turn, leads to uneven distribution of the size and shape of the resulting potassium fluorotantalate crystals, severely impacting the overall quality of the product. Although this traditional cooling crystallization technique has been widely used and recognized in industry, its limitations in cooling efficiency and the quality of the resulting crystals have become increasingly apparent, necessitating an urgent need for improvement through in-depth analysis of existing production processes and technological innovation.

[0004] To this end, improving the production efficiency of potassium fluorotantalate and the quality of the final crystals requires not only optimization in material selection and equipment design, but also the introduction of more sophisticated temperature control and fluid dynamics considerations to ensure uniform heat removal during the cooling process and the uniformity of the crystal growth environment. The use of advanced cooling technologies, such as closed-loop cooling systems and temperature gradient control, can effectively shorten the cooling time and significantly improve the uniformity and quality of the crystals. In addition, innovations in the design of the cooling tank, such as the introduction of a built-in stirring mechanism and the optimization of the tank body geometry, will also provide more ideal conditions for crystal growth. Through these process and technical improvements, not only can production efficiency be enhanced, but the performance and reliability of the resulting potassium fluorotantalate crystals in applications can also be ensured.

[0005] Against the backdrop of existing technologies, the industry has conducted a series of explorations and attempts to improve the production efficiency and final crystal quality of potassium fluorotantalate. Specifically, Zhao Mingzhi, Xiao Weichao, and Hong Gende (2014), in their research published in Rare Metals and Cemented Carbide, designed and applied a potassium fluorotantalate crystallization device with a movable cooling water jacket, aiming to optimize the cooling process. Qiu Yansong's (2014) research in Guangdong Chemical Industry focused on the details of the potassium fluorotantalate crystallization process, exploring methods to improve crystallization efficiency. Zhou Li's (2006) work focused on improving the direct yield of potassium fluorotantalate products, optimizing crystallization conditions to reduce post-processing and improve product quality. Han Jianshe, Zhao Mingzhi, and Zhou Yong (2004) shared their research on the progress of potassium fluorotantalate production processes and equipment in Rare Metals and Cemented Carbide, providing a series of strategies for improving production processes and increasing efficiency.

[0006] These studies not only deepened our understanding of the potassium fluorotantalate crystallization process but also provided valuable insights for further technological innovation. This utility model aims to draw upon and integrate these advanced research findings, specifically exploring a new solution for improving production efficiency and crystal quality by focusing on the design and application of cooling crystallization equipment. By optimizing the cooling crystallization process, this utility model aims to fundamentally improve the potassium fluorotantalate production process, thereby achieving a more efficient, economical, and environmentally friendly production model. Utility Model Content

[0007] In order to solve the above problems, the utility model provides a method for increasing the crystallization rate of potassium fluorotantalate, increasing the crystallization area of ​​potassium fluorotantalate, and improving the uniformity of potassium fluorotantalate crystals.

[0008] The technical solution adopted by this utility model is:

[0009] A device for cooling and crystallizing potassium fluorotantalate comprises a cooling tank and a plurality of pipes arranged inside the cooling tank. The pipes have a diameter range of φ30-80 mm, are closed at the bottom, and are numbered between 8 and 30 and are evenly distributed in a main pipe with a diameter of 1000 mm. The device is used to form potassium fluorotantalate crystals on the surface of the pipe after the potassium fluorotantalate solution is injected into the cooling tank, and to separate the potassium fluorotantalate crystals from the cooling tank or the pipe by knocking on the pipe.

[0010] Preferably, an inner pipe is further provided inside the pipe for achieving heat exchange between the outer pipe and the solution, causing hot air to rise, while cold air flows in from the bottom through the inner pipe to take away heat and accelerate the cooling speed.

[0011] Preferably, the inner pipe is used to mechanically introduce fresh air or cooling water to further improve cooling efficiency.

[0012] Preferably, the surface of the outer pipe is designed with a fish-scale grid with a grid size between 0.5-4 mm to increase the effective contact area when potassium fluorotantalate crystals are formed, thereby improving the crystallization efficiency and the uniformity of the crystals.

[0013] The utility model also provides a method for cooling and crystallizing potassium fluorotantalate using the above-mentioned equipment, comprising the following steps: injecting a potassium fluorotantalate solution into a cooling tank equipped with multiple pipes, forming potassium fluorotantalate crystals using the surface of the pipes, and separating the potassium fluorotantalate crystals from the cooling tank or pipes by knocking the pipes, so as to achieve rapid cooling and efficient crystallization.

[0014] The step of using the inner pipe to perform heat exchange includes causing hot air to rise through heat exchange between the outer pipe and the solution, while cold air continuously flowing in from the bottom through the inner pipe takes away the heat, thereby accelerating the cooling process.

[0015] Preferably, the method may further include mechanically introducing fresh air or cooling water through the inner pipe to further improve the cooling efficiency.

[0016] Preferably, during the cooling process, the fish-scale grid design of the external pipe is used to increase the contact area when the potassium fluorotantalate crystals are formed, so as to improve the crystallization efficiency and the uniformity of the crystals.

[0017] Through the above technical solution, the utility model achieves the following technical progress and beneficial effects:

[0018] (1) The cooling and crystallization speed of potassium fluorotantalate was significantly improved, solving the problem of slow cooling in traditional methods;

[0019] (2) It effectively increases the contact area of ​​potassium fluorotantalate crystals during the crystallization process, significantly improving the uniformity of the crystals;

[0020] (3) It has laid a solid foundation for improving the overall quality of potassium fluorotantalate products and is expected to bring about revolutionary improvements in the field of tantalum and niobium metallurgy. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The invention relates to a device for cooling and crystallizing potassium fluorotantalate according to embodiment 1 of the present invention.

[0022] Figure 2 This is the device for cooling and crystallizing potassium fluorotantalate in Example 2 of the present utility model.

[0023] Figure 3 This is the device for cooling and crystallizing potassium fluorotantalate in Example 3 of the present utility model.

[0024] Figure 4 This is the device for cooling crystallization of potassium fluorotantalate in Example 4 of the present utility model. DETAILED DESCRIPTION

[0025] The preferred embodiments of the present invention are given below in conjunction with the accompanying drawings to illustrate the technical solutions of the present invention in detail.

[0026] Example 1:

[0027] like Figure 1 As shown, a device for cooling crystallization of potassium fluorotantalate of the present invention comprises a cooling tank 100 and 8 pipes 200 arranged inside the cooling tank, the diameter of the pipe 200 is 80mm, one end of each pipe 200 is closed and formed into a hemispherical shape, the bottom of these pipes 200 is deep into the bottom of the cooling tank 100, and is evenly distributed in a main pipe with a diameter of 1000mm. When producing potassium fluorotantalate, 1000L of fluorotantalate solution is first added to the synthesis reactor, followed by addition of analytical grade potassium chloride and hydrofluoric acid to react to obtain a potassium fluorotantalate solution. After the potassium fluorotantalate solution 300 is injected into the cooling tank 100, potassium fluorotantalate crystals are formed on the surface of the pipe 200, and the potassium fluorotantalate crystals are separated from the cooling tank or the pipe by knocking the pipe 200. Through this method, the crystallization time is shortened from the original 24 hours to 20 hours, achieving rapid cooling from 90 degrees Celsius to 30 degrees Celsius.

[0028] Example 2:

[0029] like Figure 2 As shown, the same steps as in Example 1 were used, except that an inner pipe 400 with an inner diameter of 40 mm was installed inside each pipe 200 in the cooling tank 100. This configuration further shortened the crystallization time to 18 hours and reduced the mass percentage of potassium fluorotantalate crystals below an 80-mesh sieve from 15% to 10%, significantly improving the purity and uniformity of the product.

[0030] Example 3:

[0031] like Figure 3 As shown, in this embodiment, potassium fluorotantalate solution 300 is transferred to a cooling tank 100 equipped with 20 tubes with a diameter of 30 mm. Each tube 200 is fitted with an inner tube 400' with an inner diameter of 10 mm, through which air is blown. This improvement shortens the crystallization time to 16 hours and further reduces the mass percentage of potassium fluorotantalate crystals below an 80-mesh sieve to 8%, optimizing cooling efficiency and product quality.

[0032] Example 4:

[0033] like Figure 4As shown, in this embodiment, the equipment configuration of Example 3 was retained, but cooling water was introduced through inner conduit 400' instead of air. This innovation reduced the crystallization time to just 14 hours and further reduced the mass percentage of potassium fluorotantalate crystals below an 80-mesh sieve to 7%, representing a significant improvement in cooling crystallization time and product quality.

[0034] It can be seen from the above embodiments that the use of the equipment and method of the present invention not only achieves high efficiency in the production process, but also significantly improves the purity and uniformity of the final product, bringing innovative improvements to the cooling crystallization process of potassium fluorotantalate.

Claims

1. A cooling crystallization device for potassium fluorotantalate, characterized in that: The equipment includes a cooling tank and multiple pipes arranged inside the cooling tank. The diameter range of the pipes is φ30-80mm, the bottom of the pipes is closed, the number of the pipes is between 8 and 30, and they are evenly distributed in a main pipe with a diameter of 1000mm. After the potassium fluorotantalate solution is injected into the cooling tank, potassium fluorotantalate crystals are formed on the surface of the pipe, and the potassium fluorotantalate crystals are separated from the cooling tank or the pipe by knocking the pipe.

2. The cooling crystallization equipment of potassium fluorotantalate according to claim 1, characterized in that: An inner pipe is further arranged inside the pipe to realize heat exchange between the outer pipe and the solution, so as to cause the hot air to rise, and the cold air flows in from the bottom through the inner pipe to take away the heat and accelerate the cooling speed.

3. The cooling crystallization equipment of potassium fluorotantalate according to claim 2, characterized in that: The inner pipe is used to mechanically introduce fresh air or cooling water to further improve the cooling efficiency.

4. The cooling crystallization equipment of potassium fluorotantalate according to claim 2, characterized in that: The surface of the external pipe is designed with a fish-scale grid, and the grid size is between 0.5-4 mm, so as to increase the effective contact area when potassium fluorotantalate crystals are formed, thereby improving the crystallization efficiency and the uniformity of the crystals.

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