Crystallization equipment

Abstract

The utility model provides crystallization equipment. The crystallization equipment comprises at least two crystallization kettles, a material transferring assembly and a backflow assembly, the at least two crystallization kettles are configured in a manner that the crystallization kettles carry out graded crystallization on materials through gradient rising temperature along a first direction, two adjacent crystallization kettles are respectively provided with a material transfer interface and a material return interface, and the material return interface is positioned above the material transfer interface; the material transferring assembly is communicated with the material transferring interfaces of the two adjacent crystallization kettles and is used for transferring materials from one crystallization kettle to the adjacent crystallization kettles in the first direction through the material transferring interfaces; the backflow assembly is communicated with the material return interfaces of the two adjacent crystallization kettles and is used for returning materials from one crystallization kettle to the adjacent crystallization kettles along a second direction through the material return interfaces, and the second direction is opposite to the first direction. According to the crystallization equipment, multi-stage crystallization can be carried out on materials through the temperature difference, material transferring is carried out through the material transferring assembly, material returning is carried out through the backflow assembly, and multi-stage repeated crystallization is achieved.

Description

Technical Field

[0001] The present application relates to the technical field of inorganic salt concentration and crystallization preparation, and in particular to a crystallization device. Background Art

[0002] In the crystallization production of inorganic salts, the quality requirements of crystallized products are getting higher and higher. At present, some production processes are difficult to meet the demand for high-quality products. For example, in the production technology of manganese sulfate, evaporation concentration crystallization is usually used to produce manganese sulfate crystals, and the produced manganese sulfate crystals are small in particle size. The manganese sulfate crystals produced by evaporation concentration crystallization are difficult to stably grow into large-particle crystals, and cannot meet the demand for large-particle manganese sulfate crystals. Utility Model Content

[0003] The present application aims to solve at least one of the technical problems existing in the prior art. To this end, the present application proposes a crystallization device that can continuously produce large-particle inorganic salt crystals, which is beneficial to meeting the market demand for large-particle inorganic salt crystals.

[0004] According to the crystallization equipment of the embodiment of the present application, at least two crystallization kettles, a material transfer component and a reflux component are included, and the at least two crystallization kettles are configured to perform graded crystallization of the material along a first direction by stepwise increasing the temperature of each crystallization kettle, and each crystallization kettle is spaced apart from each other, and a material transfer interface and a material return interface are respectively provided on two adjacent crystallization kettles, and the material return interface is located above the material transfer interface;

[0005] The material transfer component is connected to the material transfer interfaces of two adjacent crystallization kettles. Between the two adjacent crystallization kettles, the material transfer component is used to transfer materials from one crystallization kettle to the crystallization kettle adjacent in the first direction through the material transfer interface;

[0006] The reflux component is connected to the return material interface of two adjacent crystallization kettles. Between the two adjacent crystallization kettles, the reflux component is used to return material from one crystallization kettle to the crystallization kettle adjacent along the second direction through the return material interface. The second direction is opposite to the first direction.

[0007] According to the crystallization equipment of the embodiment of the present application, at least the following beneficial effects are achieved: at least two crystallization kettles are configured to perform graded crystallization of materials by step-by-step temperature increase in each crystallization kettle along a first direction, and under the combined action of gravity and buoyancy, large-particle inorganic salt crystals can be deposited at the bottom of the crystallization kettle, and small-particle inorganic salt crystals can float on the middle and upper part of the crystallization kettle, and along the first direction, the material transfer component is connected to the material transfer interface on two adjacent crystallization kettles, and the large-particle inorganic salt crystals can be transferred from one crystallization kettle to another crystallization kettle through the material transfer component along the first direction, and the reflux component is connected to the return material interface on two adjacent crystallization kettles, and the small-particle inorganic salt crystals can be refluxed from one crystallization kettle to another crystallization kettle along the second direction to recrystallize. Thus, the crystallization equipment is conducive to the continuous growth of large-particle inorganic salt crystals and meets the market demand for large-particle crystals.

[0008] According to some embodiments of the present application, the reflux component includes a reflux pipe and a reflux valve. The reflux valve is arranged on the reflux pipe. The two ends of the reflux pipe are respectively connected to the return material interfaces on two adjacent crystallization kettles. The reflux valve is used to switch the opening and closing of the reflux pipe. The crystallization kettle is configured to be able to return material from the reflux pipe to the crystallization kettle through a pressure difference.

[0009] According to some embodiments of the present application, along the first direction, between adjacent crystallization kettles, the return material interface is divided into a return material outlet for discharging and a return material inlet for feeding, one end of the reflux pipe is connected to the return material outlet, and the other end is connected to the inlet, and the reflux valve is located on the side of the reflux pipe connected to the return material outlet.

[0010] According to some embodiments of the present application, a detection component is provided on the crystallization kettle, and the detection component is used to detect the liquid level in the crystallization kettle.

[0011] According to some embodiments of the present application, the material transfer component includes a material transfer pipeline, a material transfer pump and a material transfer valve. The material transfer pump and the material transfer valve are arranged on the material transfer pipeline. The material transfer interface is divided into a material transfer outlet for discharging material and a material transfer inlet for feeding material. Along the first direction, two adjacent crystallization kettles are respectively provided with a material transfer outlet and a material transfer inlet. One end of the material transfer pipeline is connected to the material transfer outlet, and the other end of the material transfer pipeline is connected to the material transfer inlet.

[0012] According to some embodiments of the present application, the number of crystallization kettles is three, and the crystallization kettles are spaced apart from each other along the first direction.

[0013] According to some embodiments of the present application, a heating structure is connected to the crystallization kettle, the heating structure is located outside the crystallization kettle, and the heating structure is used to heat the crystallization kettle.

[0014] According to some embodiments of the present application, a heating structure is connected to the crystallization kettle at the end along the first direction.

[0015] According to some embodiments of the present application, an agitator is provided in the crystallization kettle, the agitator is connected to the crystallization kettle, and the agitator is used to stir the material in the crystallization kettle.

[0016] According to some embodiments of the present application, the return material interface is divided into a return material outlet for discharging material and a return material inlet for feeding material. Along the first direction, two adjacent crystallization kettles are respectively provided with a return material outlet and a return material inlet, and the return material outlet is located above the return material inlet. The return material outlet, the reflux assembly and the return material inlet are configured to be able to reflux material along the second direction.

[0017] Additional aspects and advantages of the present application will be given in part in the description below, and in part will become apparent from the description below, or will be learned through the practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The present application is further described below with reference to the accompanying drawings and embodiments, wherein:

[0019] Figure 1 This is a schematic diagram of the structure of the two-stage crystallization of the crystallization equipment in the embodiment of the present application;

[0020] Figure 2 This is a schematic diagram of the structure of the three-stage crystallization of the crystallization equipment in the embodiment of the present application;

[0021] Figure 3 This is a schematic diagram of the structure of the four-stage crystallization of the crystallization equipment in the embodiment of the present application;

[0022] Figure 4 Another structural schematic diagram of the three-stage crystallization of the crystallization equipment of the embodiment of the present application;

[0023] Figure 5 This is another structural schematic diagram of the three-stage crystallization of the crystallization equipment in the embodiment of the present application.

[0024] Reference numerals: crystallization kettle 100, primary crystallization kettle 101, secondary crystallization kettle 102, tertiary crystallization kettle 103, quaternary crystallization kettle 104, material transfer interface 110, material transfer inlet 111, material transfer outlet 112, return material interface 120, return material inlet 121, return material outlet 122, detection element 130, heating structure 140, stirrer 150, material inlet 160, and material outlet 170;

[0025] Material transfer assembly 200, material transfer pipeline 210, material transfer pump 220, material transfer valve 230;

[0026] Reflux assembly 300 , reflux pipe 310 , reflux valve 320 . DETAILED DESCRIPTION

[0027] The embodiments of the present application are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present application, and cannot be understood as limiting the present application.

[0028] In the description of the present application, it should be understood that descriptions involving orientation, such as up, down, front, back, left, right, etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0029] In the description of this application, "several" means more than one, "more" means more than two, "greater than", "less than", "exceed", etc. are understood to exclude the number itself, and "above", "below", "within", etc. are understood to include the number itself. If there is a description of "first" or "second", it is only used for the purpose of distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0030] In the description of this application, unless otherwise clearly defined, terms such as setting, installing, connecting, etc. should be understood in a broad sense, and technicians in the relevant technical field can reasonably determine the specific meanings of the above terms in this application based on the specific content of the technical solution.

[0031] In the description of the present application, the description with reference to the terms "one embodiment", "some embodiments", "illustrative embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.

[0032] The following is an introduction to the embodiments of the present application in conjunction with the accompanying drawings:

[0033] refer to Figures 1 to 3According to the crystallization equipment of the embodiment of the present application, at least two crystallization kettles 100 are configured to perform graded crystallization of materials by step-up temperature in each crystallization kettle 100 along the first direction, each crystallization kettle 100 is spaced apart from each other, and a material transfer interface 110 and a material return interface 120 are respectively provided on two adjacent crystallization kettles 100, and the material return interface 120 is located above the material transfer interface 110 along the third direction. It should be understood that in the crystallization kettles 100 at different temperatures, the inorganic salt material has different solubility. Taking manganese sulfate as an example, within a certain temperature range, as the temperature increases, the solubility of manganese sulfate will decrease. Based on the solubility characteristics of manganese sulfate, along the first direction, the temperature in each crystallization kettle 100 distributed at intervals is configured to be stepped up. Along the first direction, the manganese sulfate solution can pass through each crystallization kettle 100 in sequence, and graded crystallization is performed in different crystallization kettles 100, which is beneficial to the growth of crystals.

[0034] The crystallization equipment also includes a material transfer component 200 and a reflux component 300. Along a first direction, the material transfer component 200 is connected in sequence to the material transfer interfaces 110 of two adjacent crystallization kettles 100, and the reflux component 300 is connected in sequence to the return material interfaces 120 of two adjacent crystallization kettles 100. Between two adjacent crystallization kettles, the material transfer component 200 is used to transfer material from one crystallization kettle 100 to the crystallization kettle 100 adjacent to the first direction through the material transfer interface 110, and the reflux component 300 is used to return material from one crystallization kettle 100 to the crystallization kettle 100 adjacent to the second direction through the return material interface 120. The first direction and the second direction are opposite, and the third direction is perpendicular to the first direction.

[0035] Under the action of gravity, along the third direction, the large crystals crystallized are easily deposited at the bottom of the crystallization kettle 100, and the small crystals are easily floated in the solution and located in the middle and upper part of the crystallization kettle 100. Specifically, two adjacent crystallization kettles 100 are configured to obtain large crystals from the material transfer interface 110 in one crystallization kettle 100 along the first direction through the material transfer component 200, and transfer the large crystals to the material transfer interface 110 of another crystallization kettle 100, thereby realizing the transfer of large crystals between adjacent crystallization kettles 100. The two adjacent crystallization kettles 100 are configured to increase the temperature stepwise along the first direction. Taking manganese sulfate as an example, manganese sulfate has the characteristic of decreasing solubility as the temperature increases, so that the crystals can crystallize and grow again, which is beneficial to increasing the growth size of the crystals.

[0036] refer to Figure 1In some embodiments, the crystallization equipment includes a crystallization kettle 100, which can be divided into a primary crystallization kettle 101 and a secondary crystallization kettle 102. Along the first direction, the primary crystallization kettle 101 and the secondary crystallization kettle 102 are spaced apart from each other, and a material transfer interface 110 and a material return interface 120 are provided on the primary crystallization kettle 101, and a material transfer interface 110 and a material return interface 120 are provided on the secondary crystallization kettle 102. Both ends of the material transfer component 200 are respectively connected to the material transfer interface 110 on the primary crystallization kettle 101 and the material transfer interface 110 on the secondary crystallization kettle 102, and both ends of the reflux component 300 are respectively connected to the material return interface 120 on the primary crystallization kettle 101 and the material return interface 120 on the secondary crystallization kettle 102, thereby realizing the connection between the primary crystallization kettle 101 and the secondary crystallization kettle 102.

[0037] Among them, the first-level crystallization kettle 101 is also provided with a feed inlet 160 for adding materials. The material located in the first-level crystallization kettle 101 undergoes the first crystallization in the first-level crystallization kettle 101. Along the third direction, the large-particle crystals crystallized are deposited at the bottom of the first-level crystallization kettle 101, and the small-particle crystals float up and are located in the middle and upper part of the first-level crystallization kettle 101. The material transfer interface 110 is located at the bottom of the first-level crystallization kettle 101. The material transfer component 200 can transfer the large-particle crystals from the material transfer interface 110 on the first-level crystallization kettle 101 to the material transfer interface 110 on the secondary crystallization kettle 102. Compared with the first-level crystallization kettle 101, the secondary crystallization kettle 102 is configured with a higher temperature, and the material from the first-level crystallization kettle 101 can be crystallized again in the secondary crystallization kettle 102. Similarly, under the action of gravity, along the third direction, large-particle crystals are deposited at the bottom of the secondary crystallization kettle 102, and small-particle crystals float up and are located in the middle and upper part of the secondary crystallization kettle 102. Through the reflux assembly 300, the small-particle crystals in the middle and upper part of the secondary crystallization kettle 102 can be refluxed to the primary crystallization kettle 101. The temperature in the primary crystallization kettle 101 is relatively low compared to the temperature in the secondary crystallization kettle 102. The crystals of small particles refluxed to the primary crystallization kettle 101 can be dissolved again in the primary crystallization kettle 101, and with the replenishment of the materials in the primary crystallization kettle 101, the crystals of the dissolved small particles can be recrystallized and precipitated. It should be understood that a part of the re-dissolved small-particle crystals is recrystallized into large-particle crystals and deposited at the bottom of the primary crystallization kettle 101, and another part of the re-crystallized small-particle crystals floats in the middle and upper part of the primary crystallization kettle 101, ready to be dissolved again for deposition, thereby, being conducive to continuous crystallization of large-particle crystals and achieving stable production of large-particle crystals.

[0038] It should be noted that when the material transfer component 200 transfers materials, the materials it transfers include large-particle crystals and solutions, and when the reflux component 300 refluxes, the materials it refluxes include small-particle crystals and solutions. The secondary crystallization kettle 102 is provided with a discharge port 170 for discharging materials to obtain large-particle crystals, and the large-particle crystals and part of the solution after two-stage crystallization flow out from the discharge port 170 of the secondary crystallization kettle 102 and are dehydrated to obtain large-particle crystals. Therefore, in the process of producing large-particle crystals, the material in the primary crystallization kettle 101 should be gradually reduced, and the material needs to be continuously replenished through the feed port 160 on the primary crystallization kettle 101 to keep the two-stage reciprocating crystallization going on.

[0039] refer to Figure 2 In some embodiments, the crystallization equipment includes a first-stage crystallization kettle 101, a second-stage crystallization kettle 102 and a third-stage crystallization kettle 103 which are spaced apart from each other along a first direction, each crystallization kettle 100 is provided with a material transfer interface 110 and a material return interface 120, the first-stage crystallization kettle 101 is also provided with a material inlet 160, and the third-stage crystallization kettle 103 is also provided with a material outlet 170, and the two ends of the material transfer component 200 are respectively connected to the material transfer interfaces 110 on the two adjacent crystallization kettles 100, and the two ends of the reflux component 300 are respectively connected to the material return interfaces 120 on the two adjacent crystallization kettles 100, and the first-stage crystallization kettle 101, the second-stage crystallization kettle 102 and the third-stage crystallization kettle 103 are respectively connected to the material return interface 120 on the two adjacent crystallization kettles 100. The first temperature, the second temperature and the third temperature are respectively corresponding to the first crystallization kettle 103, the first temperature is lower than the second temperature, and the second temperature is lower than the third temperature, so that the inorganic salt crystals can be multi-stage crystallized in the first crystallization kettle 101, the second crystallization kettle 102 and the third crystallization kettle 103. The crystals crystallized in the crystallization kettle 100 can be divided into two parts: floating and deposited. Small-particle crystals float and large-particle crystals deposit. The material transfer component 200 can transfer the large-particle crystals deposited in the first crystallization kettle 101 to the second crystallization kettle 102, and transfer the crystals deposited in the second crystallization kettle 102 to the third crystallization kettle 103. Along the second direction, the reflux component 300 can reflux the small-particle crystals floating in the second crystallization kettle 102 to the first crystallization kettle 101 for redissolution and recrystallization, and reflux the small-particle crystals floating in the third crystallization kettle 103 to the second crystallization kettle 102 for redissolution and recrystallization, which is beneficial to improve the yield of large-particle crystals.

[0040] It should be noted that, along the first direction, the crystallization equipment may include multiple crystallization kettles 100. Among the multiple crystallization kettles 100, along the first direction, the crystallization kettle 100 located at the first stage is provided with an inlet 160, and the crystallization kettle 100 located at the last stage is provided with a discharge port 170, and each crystallization kettle 100 is provided with a material transfer interface 110 and a return material interface 120. The material is added at the inlet 160 on the crystallization kettle 100 of the first stage, and the large-particle crystals after crystallization at each stage are taken out at the discharge port 170 on the crystallization kettle 100 of the last stage.

[0041] refer to Figures 1 to 3 In some embodiments, the reflux assembly 300 includes a reflux pipe 310 and a reflux valve 320. The reflux valve 320 is disposed on the reflux pipe 310. Both ends of the reflux pipe 310 are respectively connected to the return material interfaces 120 on two adjacent crystallization kettles 100. The reflux valve 320 is used to switch the opening and closing of the reflux pipe 310. The crystallization kettle 100 is configured to be able to return material from the reflux pipe 310 to the crystallization kettle 100 through a pressure difference. Therefore, the adjacent crystallization kettles 100 are configured to have different pressures. For example, along the first direction, the pressure in each crystallization kettle 100 increases stepwise, so that along the second direction, the small particle crystals can be refluxed in the adjacent crystallization kettle 100 through the reflux pipe 310 and the reflux valve 320 through the pressure difference to dissolve and crystallize again, without the need to additionally set up a power pump, which is beneficial to realize the one-way automatic reflux of the small particle crystals along the second direction and improve the output rate of the large particle crystals.

[0042] It should be understood that the reflux valve 320 has unidirectional conductivity. Therefore, along the second direction, the reflux valve 320 only allows the material to reflux from the crystallization kettle 100 with a higher pressure to the crystallization kettle 100 with a lower pressure, thereby ensuring that the crystallization kettle 100 with a higher pressure has a higher proportion of large-particle crystals. The crystallization reflux through the multi-stage crystallization kettle 100 is beneficial to the continuous production of large-particle crystals.

[0043] refer to Figure 2 and Figure 4In some embodiments, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102 and a tertiary crystallization kettle 103. Along the first direction, the three crystallization kettles 100 are spaced apart from each other. Each crystallization kettle 100 is configured to increase the temperature and pressure in a stepwise manner, thereby forming a temperature difference and a pressure difference between adjacent crystallization kettles 100. Taking manganese sulfate as an example, within a certain temperature range, the solubility of manganese sulfate decreases with the increase of temperature. Based on the solubility characteristics of manganese sulfate, after manganese sulfate crystals are crystallized in the primary crystallization kettle 101, most of the materials deposited at the bottom of the primary crystallization kettle 101 are transferred to the secondary crystallization kettle 102 through the material transfer component 200. The transferred crystals include large-particle crystals and part of the solution. The secondary crystallization kettle 102 receives the solution from the primary crystallization kettle 101 and crystallizes again. The large-particle crystals are deposited at the bottom of the secondary crystallization kettle 102, and the small-particle crystals float on the middle and upper part of the secondary crystallization kettle 102. The reflux component 300 refluxes the crystals located in the middle and upper part of the secondary crystallization kettle 102 to the primary crystallization kettle 101. Similarly, the material at the bottom of the secondary crystallization kettle 102 is transferred to the tertiary crystallization kettle 103 through the material transfer component 200, and is crystallized again in the tertiary crystallization kettle 103. Similarly, most of the deposited at the bottom of the tertiary crystallization kettle 103 should be large-particle crystals, and most of the small-particle crystals float on the tertiary crystallization kettle 103. Through the pressure difference between the tertiary crystallization kettle 103 and the secondary crystallization kettle 102, the reflux valve 320 and the reflux pipe 310 can realize the reflux of the small-particle crystals, and the refluxed small-particle crystals are re-dissolved and recrystallized, which is beneficial to the continuous output of large-particle crystals of manganese sulfate.

[0044] It should be noted that the crystals deposited at the bottom of the crystallization kettle 100 include large-grain crystals and small-grain crystals. The large-grain crystals occupy the majority of the crystals, and the majority of the crystals located in the upper middle portion of the crystallization kettle 100 should be small-grain crystals.

[0045] refer to Figure 1 and Figure 2In some embodiments, the reflux component 300 includes a reflux pipe 310 and a reflux valve 320. The reflux valve 320 is disposed on the reflux pipe 310 between two adjacent crystallization kettles 100. The return material interface 120 is divided into a return material outlet 122 for discharging and a return material inlet 121 for feeding. Along a first direction, one end of the reflux pipe 310 is connected to the return material outlet 122, and the other end is connected to the return material inlet 121. The reflux pipe 310 is used to reflux the material along a second direction opposite to the first direction, so that the material refluxes between the two adjacent crystallization kettles 100. Among them, the reflux valve 320 is located on the side of the reflux pipe 310 connected to the return material outlet 122. Since the adjacent crystallization kettles 100 are configured with a temperature difference, the reflux pipe 310 is connected to the two adjacent crystallization kettles 100. The reflux valve 320 divides the reflux pipe 310 into two sections with higher temperature and lower temperature. The reflux valve 320 is located on the side close to the return material outlet 122, so that the section with higher temperature of the reflux pipe 310 is shorter than the section with lower temperature. The refluxed material contains small particle crystals and solution, and the crystals can be redissolved when they reflux to the section with lower temperature. Therefore, the reflux valve 320 is located on the side close to the return material outlet 122, so that the reflux pipe 310 can include a longer pipe section with lower temperature, thereby preventing crystals from blocking the reflux pipe 310 during reflux, ensuring the normal reflux of materials, and being beneficial to the continuous and stable output of large particle crystals.

[0046] It should be noted that the crystallization equipment can also be used to crystallize other inorganic salt crystals. The temperature difference in adjacent crystallization kettles 100 changes according to the solubility characteristics of the inorganic salt, and the position of the above-mentioned reflux valve 320 can be changed according to the type of crystallized inorganic salt to prevent blockage of the reflux pipe 310.

[0047] refer to Figure 2 In some embodiments, the crystallization kettle 100 is connected with a detection member 130, which may be a liquid level detector. The detection member 130 is used to detect the liquid level of the material in the crystallization kettle 100. Specifically, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102, and a tertiary crystallization kettle 103. Each crystallization kettle 100 is connected with a detection member 130. The detection member 130 can detect the liquid level of the material in each crystallization kettle 100, so as to balance the liquid level in each crystallization kettle 100 and avoid the liquid level in any crystallization kettle 100 being too high or too low. It should be noted that the adjacent crystallization kettles 100 at each level are connected through the reflux assembly 300, the reflux assembly 300 includes a reflux pipe 310 and a reflux valve 320, the reflux valve 320 is arranged on the reflux pipe 310, and the reflux valve 320 is configured to be able to adjust the opening. The adjacent crystallization kettles 100 at each level are also connected through the material transfer assembly 200, and the material transfer assembly 200 is used to transfer materials between adjacent crystallization kettles 100. Through the coordination of the reflux assembly 300 and the material transfer assembly 200, the material transfer and reflux in each crystallization kettle 100 can achieve dynamic balance.

[0048] For example, the primary crystallization kettle 101 adds materials through the feed port 160, and also refluxes the materials in the secondary crystallization kettle 102 to the primary crystallization kettle 101 through the reflux component 300. At the same time, the material transfer component 200 transfers the materials in the primary crystallization kettle 101 to the secondary crystallization kettle 102. The detection component 130 is used to detect the liquid level in the primary crystallization kettle 101, so that the liquid level in the primary crystallization kettle 101 is at the same height, that is, the amount of material added through the feed port 160 and the return material inlet 121 is the same as the amount of material flowing out of the material transfer outlet 112.

[0049] refer to Figures 1 to 3 In some embodiments, the material transfer assembly 200 includes a material transfer pipeline 210, a material transfer pump 220 and a material transfer valve 230. The material transfer pump 220 and the material transfer valve 230 are arranged on the material transfer pipeline 210. A material transfer inlet 111 and a material transfer outlet 112 are respectively arranged on two adjacent crystallization kettles 100 along the first direction. One end of the material transfer pipeline 210 is connected to the material transfer inlet 111, and the other end of the material transfer pipeline 210 is connected to the material transfer outlet 112. The material transfer valve 230 is arranged on the material transfer pipeline 210. The material transfer valve 230 can adjust the opening, thereby regulating the material transfer rate of the material transfer pump 220, so as to achieve a dynamic balance between the feeding and discharging in each crystallization kettle 100, so as to maintain the continuous growth of the crystal.

[0050] It should be understood that, due to the pressure difference in each crystallization kettle 100, it is necessary to use the material transfer pump 220 to achieve transfer along the first direction from the crystallization kettle 100 with lower pressure to the crystallization kettle 100 with higher temperature. The transferred material is a mixture of crystals and solution, most of which are large-particle manganese sulfate crystals deposited at the bottom of the crystallization kettle 100.

[0051] refer to Figure 2 In some embodiments, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102 and a tertiary crystallization kettle 103. Along the first direction, there is a gap between the primary crystallization kettle 101, the secondary crystallization kettle 102 and the tertiary crystallization kettle 103. Two adjacent crystallization kettles 100 are connected through a material transfer component 200 and a reflux component 300, and a temperature difference and a pressure difference are configured between the primary crystallization kettle 101, the secondary crystallization kettle 102 and the tertiary crystallization kettle 103. Along the first direction, the primary crystallization kettle 101, the secondary crystallization kettle 102 and the tertiary crystallization kettle 103 are configured to increase the temperature and pressure step by step.

[0052] It should be understood that the solubility of the crystals in the primary crystallization kettle 101, the secondary crystallization kettle 102 and the tertiary crystallization kettle 103 is different. The crystal solution is added to the primary crystallization kettle 101 at the feed inlet 160 of the primary crystallization kettle 101. The crystal solution crystallizes at a first temperature in the primary crystallization kettle 101. Manganese sulfate crystals are deposited at the bottom of the primary crystallization kettle 101 along the third direction. The material transfer component 200 transfers the material deposited at the bottom of the primary crystallization kettle 101 to the secondary crystallization kettle 102. The secondary crystallization kettle 102 has a second temperature, and the second temperature is higher than the first temperature. The solubility of the crystal changes with temperature, and the material transferred to the secondary crystallization kettle 102 is crystallized again.

[0053] Along the third direction, large-particle crystals are deposited at the bottom of the secondary crystallization kettle 102, and small-particle crystals float on the upper part of the secondary crystallization kettle 102. The small-particle crystals located on the upper part of the secondary crystallization kettle 102 are refluxed to the primary crystallization kettle 101 through the reflux component 300 to be redissolved and recrystallized. The material transfer component 200 transfers the material deposited at the bottom of the secondary crystallization kettle 102 to the tertiary crystallization kettle 103. The tertiary crystallization kettle 103 has a third temperature, and the third temperature is higher than the second temperature. The material transferred to the tertiary crystallization kettle 103 is crystallized again. Along the third direction, large-particle crystals are deposited at the bottom of the tertiary crystallization kettle 103, and small-particle crystals float on the upper part of the tertiary crystallization kettle 103. The small crystals located on the upper part of the tertiary crystallization kettle 103 are refluxed to the secondary crystallization kettle 102 through the reflux component 300 to be redissolved and recrystallized.

[0054] Through the discharge port 170 at the bottom of the tertiary crystallization kettle 103, the crystals deposited at the bottom of the tertiary crystallization kettle 103 can be taken out and dehydrated to obtain large-particle crystals. Thus, large-particle crystals can be produced continuously and stably to meet the demand for large-particle crystals.

[0055] refer to Figure 2 In some embodiments, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102, and a tertiary crystallization kettle 103. A heating structure 140 is provided on each level of the crystallization kettle 100. The heating structure 140 is located outside the crystallization kettle 100 and is used to heat the crystallization kettle 100. The heating structures 140 on each level of the crystallization kettle 100 are independent of each other and can heat each level of the crystallization kettle 100 to different temperatures. For example, along the first direction, the primary crystallization kettle 101, the secondary crystallization kettle 102, and the tertiary crystallization kettle 103 are configured to be heated by the heating structure 140 to a state where the temperature is gradually increased. Thus, taking manganese sulfate as an example, the solubility of manganese sulfate crystals in the primary crystallization kettle 101, the secondary crystallization kettle 102, and the tertiary crystallization kettle 103 is successively reduced, so as to achieve multi-stage precipitation of manganese sulfate crystals.

[0056] refer to Figure 4In some embodiments, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102 and a tertiary crystallization kettle 103. A heating structure 140 is provided on the tertiary crystallization kettle 103. The heating structure 140 can heat the tertiary crystallization kettle 103. The return material outlet 122 on the tertiary crystallization kettle 103 is connected to the reflux component 300. The reflux component 300 is connected to the return material inlet 121 on the secondary crystallization kettle 102. The material in the tertiary crystallization kettle 103 can be refluxed to the secondary crystallization kettle 102 through the reflux component 300. It should be understood that in the process of material reflux, the material will lose part of the heat. Therefore, the temperature of the material will decrease when it is refluxed from the tertiary crystallization kettle 103 to the secondary crystallization kettle 102. Similarly, the return material outlet 122 on the secondary crystallization kettle 102 is also connected to the return material inlet 121 on the primary crystallization kettle 101 through the reflux component 300. The temperature of the material in the secondary crystallization kettle 102 will also decrease when it is refluxed to the primary crystallization kettle 101. Thus, a temperature difference can be formed in the first-stage crystallization kettle 101, the second-stage crystallization kettle 102 and the third-stage crystallization kettle 103, and the crystals have different solubilities at different temperatures. Taking manganese sulfate as an example, within a certain temperature range, the higher the temperature, the lower the solubility. By arranging a heating structure 140 on the third-stage crystallization kettle 103, multi-stage crystallization of the manganese sulfate solution can be achieved, which is beneficial to improving the quality of the crystals.

[0057] refer to Figures 1 to 3 In some embodiments, a stirrer 150 is provided in the crystallization kettle 100, and the stirrer 150 is connected to the crystallization kettle 100. The stirrer 150 can stir in the crystallization kettle 100, which is beneficial to the re-dissolution of the refluxed material. At the same time, in the polyionic liquid environment, stirring can also easily accelerate the growth of crystals and increase the crystallization rate.

[0058] refer to Figure 5 In some embodiments, the feed interface 120 is divided into a feed outlet 122 for discharging and a feed inlet 121 for feeding. Along the first direction, two adjacent crystallization kettles are provided with a feed outlet 122 and a feed inlet 121, respectively. The feed outlet 122 is located above the feed inlet 121. The feed outlet 122, the reflux assembly 300 and the feed inlet 121 are configured to reflux materials along the second direction. Since the feed outlet 122 is located above the feed inlet 121, the crystallized material can be prevented from flowing back along the first direction, so that the crystallized material can flow back along the second direction more smoothly.

[0059] Specifically, the crystallization equipment includes a primary crystallization kettle 101, a secondary crystallization kettle 102 and a tertiary crystallization kettle 103. The primary crystallization kettle 101 is provided with a feed inlet 160 and a return material inlet 121, the secondary crystallization kettle 102 is provided with a return material inlet 121 and a return material outlet 122, and the tertiary crystallization kettle 103 is provided with a discharge port 170 and a return material outlet 122. Along the third direction, the return material inlet 121 on the primary crystallization kettle 101 is located below the return material outlet 122 on the secondary crystallization kettle 102, and the return material inlet 121 on the secondary crystallization kettle 102 is located below the return material outlet 122 on the tertiary crystallization kettle 103. The return material outlets 122 on the crystallization kettles 100 at each level may be at the same height. Along the first direction, the return material inlet 121 on the first crystallization kettle 101 is connected with the return material outlet 122 on the second crystallization kettle 102 through the reflux component 300, and the return material inlet 121 on the second crystallization kettle 102 is connected with the return material outlet 122 on the tertiary crystallization kettle 103 through the reflux component 300. The materials located in the crystallization kettles 100 at each level can be refluxed between adjacent crystallization kettles 100 along the second direction through the reflux component 300. The second direction is opposite to the first direction. The material reflux can reflux the small particle crystals located in the upper part of the crystallization kettle 100 to the adjacent crystallization kettle 101 for re-dissolution and crystallization, which is beneficial to increase the proportion of large particle crystals in the crystal product.

[0060] Along the third direction, the backfeed inlet 121 is located below the backfeed outlet 122 to allow the material to reflux more smoothly. It should be understood that along the third direction, the bottom of the crystallization kettle 100 is precipitated with crystals that have crystallized. Relative to other positions of the crystallization kettle 100, the solution at the bottom of the crystallization kettle 100 is closer to a saturated solution, and has a poor dissolving ability for the refluxed small-particle crystals. Therefore, the position of the backfeed inlet 121 should not be too low. Along the third direction, the backfeed inlet 121 is located above the transfer outlet 112 to ensure that the refluxed small-particle crystals are redissolved in the middle and upper part of the crystallization kettle 100, which is beneficial to improve the dissolution rate, thereby improving the production efficiency of large-particle crystals.

[0061] It should be noted that the above-mentioned material can be a barium sulfate solution or other types of inorganic salt solutions. The temperature difference and pressure difference in each stage of the crystallization kettle 100 can be adaptively adjusted according to the different types of inorganic salts to achieve multi-stage reflux repeated crystallization, which is beneficial to obtain large-particle inorganic salt crystals.

[0062] The embodiments of the present application are described in detail above in conjunction with the accompanying drawings, but the present application is not limited to the above embodiments. Various changes can be made within the knowledge of ordinary technicians in the relevant technical field without departing from the purpose of the present application. In addition, the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.

Claims

1. A crystallization device, characterized in that: include: At least two crystallization kettles are configured to perform graded crystallization of the material along a first direction by stepwise increasing the temperature of each crystallization kettle, each crystallization kettle is spaced apart from each other, and a material transfer interface and a material return interface are respectively provided on two adjacent crystallization kettles, and the material return interface is located above the material transfer interface; A material transfer component, connected to the material transfer interfaces of two adjacent crystallization kettles, between the two adjacent crystallization kettles, the material transfer component is used to transfer materials from one crystallization kettle to the crystallization kettle adjacent along the first direction through the material transfer interface; A reflux component is connected to the return material interface of two adjacent crystallization kettles. Between the two adjacent crystallization kettles, the reflux component is used to return material from one crystallization kettle to the crystallization kettle adjacent to it along a second direction through the return material interface, and the second direction is opposite to the first direction.

2. The crystallization device according to claim 1, characterized in that The reflux component includes a reflux pipe and a reflux valve, wherein the reflux valve is arranged on the reflux pipe, and the two ends of the reflux pipe are respectively connected to the return material interfaces on the two adjacent crystallization kettles, and the reflux valve is used to switch the opening and closing of the reflux pipe, and the crystallization kettle is configured to be able to return material from the reflux pipe to the crystallization kettle through a pressure difference.

3. The crystallization device according to claim 2, characterized in that Along the first direction, between adjacent crystallization kettles, the return material interface is divided into a return material outlet for discharging and a return material inlet for feeding, one end of the reflux pipe is connected to the return material outlet, and the other end is connected to the inlet, and the reflux valve is located on the side of the reflux pipe connected to the return material outlet.

4. The crystallization device according to claim 1, characterized in that The crystallization kettle is provided with a detection component, and the detection component is used to detect the liquid level in the crystallization kettle.

5. The crystallization device according to claim 1, characterized in that The material transfer component includes a material transfer pipeline, a material transfer pump and a material transfer valve. The material transfer pump and the material transfer valve are arranged on the material transfer pipeline. The material transfer interface is divided into a material transfer outlet for discharging material and a material transfer inlet for feeding material. Along the first direction, the material transfer outlet and the material transfer inlet are respectively provided on two adjacent crystallization kettles. One end of the material transfer pipeline is connected to the material transfer outlet, and the other end of the material transfer pipeline is connected to the material transfer inlet.

6. The crystallization device according to claim 1, characterized in that The number of the crystallization kettles is three, and the crystallization kettles are spaced apart from each other along the first direction.

7. The crystallization device according to claim 1, characterized in that The crystallization kettle is connected with a heating structure, which is located outside the crystallization kettle and is used to heat the crystallization kettle.

8. The crystallization device according to claim 7, characterized in that The heating structure is connected to the crystallization kettle at the end along the first direction.

9. The crystallization device according to claim 1, characterized in that A stirrer is arranged in the crystallization kettle, the stirrer is connected to the crystallization kettle, and the stirrer is used to stir the material in the crystallization kettle.

10. The crystallization device according to claim 1, characterized in that The return material interface is divided into a return material outlet for discharging material and a return material inlet for feeding material. Along the first direction, the return material outlet and the return material inlet are respectively provided on two adjacent crystallization kettles, and the return material outlet is located above the return material inlet. The return material outlet, the reflux assembly and the return material inlet are configured to be able to reflux the material along the second direction.

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