CN217887033U - Multistage circulation crystallization system device - Google Patents
Multistage circulation crystallization system device Download PDFInfo
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- CN217887033U CN217887033U CN202221189770.1U CN202221189770U CN217887033U CN 217887033 U CN217887033 U CN 217887033U CN 202221189770 U CN202221189770 U CN 202221189770U CN 217887033 U CN217887033 U CN 217887033U
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Abstract
The utility model provides a multistage circulating crystallization system device, which comprises at least two circulating crystallization devices which are connected in series in sequence and have the same structure; the circulating crystallization device comprises a shell, wherein a flow guide structure of a funnel structure is arranged in the shell, the flow guide structure comprises a flow guide conical section and a flow guide pipe section which are sequentially butted from top to bottom, and the edge of the large end face of the flow guide conical section is butted with the inner wall of the shell in the circumferential direction; the shell cavity of water conservancy diversion conic section top forms and mixes the storehouse, the shell cavity of water conservancy diversion pipeline section periphery forms the crystallization storehouse, the inner chamber bottom of casing is provided with agitating unit, feed inlet and at least one circulation entry have been seted up to the outer wall in mixed storehouse, at least one circulation export has been seted up on the outer wall upper portion in crystallization storehouse, circulation entry and circulation export communicate through external circulation pipeline, the discharge gate has been seted up to the outer wall bottom in crystallization storehouse, the discharge gate inserts next stage circulation crystallization device's circulation pipeline or next stage circulation crystallization device's feed inlet.
Description
Technical Field
The utility model belongs to the technical field of the crystallization, a multistage circulation crystal system device is related to.
Background
In the production of the pharmaceutical and chemical industries, the crystallization process is divided into two modes of continuous crystallization and intermittent crystallization according to the operation mode; the crystallization process is further classified into reaction crystallization, evaporation crystallization, cooling crystallization, and elution crystallization according to the physical and chemical properties such as solubility of the system. The intermittent crystallization process is a crystallization process of adding raw materials at one time, then obtaining crystal grains by adopting different crystallization methods, and finally separating the crystal grains from mother liquor at one time, and is suitable for products with small annual output. In order to regulate and control the particle size of the product, the intermittent crystallization process can be carried out along with time, and technological parameter conditions such as evaporation rate, cooling rate, feeding rate, seed crystal adding and the like of the material are regulated and changed, so that the proper supersaturation degree is controlled, and the quality indexes such as the particle size, the bulk density and the like of the final product are optimized. Due to the characteristics of the operation mode of the intermittent crystallization, process operation control parameters change along with time, the influence factors are multiple, the coupling of control variables is strong, the experience and the regulation and control precision of operators are greatly depended, the product quality and the process yield are unstable, the batch difference is large, the problems of poor product consistency, uneven grain size and the like are caused, and the requirements of customers cannot be met. Because the batch crystallization operation is discontinuous, the production and preparation efficiency is not high, and the quantity of equipment or the occupied area is large.
The continuous crystallization is a crystallization process for continuously feeding materials into a crystallizer and continuously obtaining products, is suitable for a large-scale industrial crystallization process, can be realized by one or more crystallization devices connected in series, each crystallization device is called as a first stage, the technological parameters of each stage of crystallization device are constant and do not change along with time, and the crystallization process is more stable and easy to control, so that the stability and consistency of the quality of crystal grain products are ensured, and the influence of human factors on the crystallization process is greatly reduced. Because the production efficiency of the continuous crystallization process is high, the volume or the quantity of equipment in the crystallization process can be greatly reduced, so that the crystallization process which originally needs a plurality of intermittent crystallizers becomes only one set of continuous crystallization system. And due to continuous production, the influence of manual operation on crystal grains can be reduced, the difference of products in different batches is reduced, and the aim of stably controlling the production process and the product quality is fulfilled.
CN108939599A discloses a self-circulation crystallizer and a multistage continuous crystallization method, the crystallizer comprises from top to bottom: the device comprises a kettle head, an upper cylinder, a middle cylinder and a bottom reducing cylinder with a W bottom; a steam outlet and/or a charging opening are/is arranged on the kettle head, and an annular spraying pipe is arranged at the lower part of the kettle head; a middle straight cylinder section is arranged in the middle round cylinder body, a guide cylinder is arranged in the middle straight cylinder section, and a stirrer is arranged in the guide cylinder; the diameter of the middle cylinder body is larger than that of the upper cylinder body, and the diameter of the upper cylinder body is larger than that of the middle straight cylinder section; the lower part of the upper cylinder body and the upper part of the middle cylinder body are respectively connected with the top circumference of the middle straight cylinder section through the reducing transition section, and the W-shaped bottom is provided with a discharge hole.
CN2855495U discloses a multistage sectional continuous crystallizer, the upper and lower ends of a crystallization column are respectively provided with an inlet and an outlet of crystallization liquid, a jacket is arranged outside the crystallization column, and the upper and lower ends of the jacket are provided with an inlet and an outlet of cold and hot media. A constant temperature filter is arranged between every two stages of crystallization columns in the optimization scheme, the constant temperature filter is divided into an upper section structure and a lower section structure, the two sections are connected in a sealing mode and are respectively connected with the upper section filter and the lower section filter in a sealing mode. The bottom of the constant temperature filter is provided with a circular flat plate, holes are uniformly formed, and filter paper or filter cloth is placed on the circular flat plate. The middle lower end of the crystallization column is provided with a thermo-well tube.
CN209778705U discloses a system for continuously crystallizing calcium gluconate, which comprises an MVR evaporator, a three-level vacuum flash crystallizer, a steam jet vacuum pump, a hybrid condenser, a heat exchanger, a slurry tank, a centrifuge, a granulator and a dryer, and the process steps are as follows: and (3) concentrating the supernatant of the calcium gluconate in an MVR evaporator until the concentration of the material is 50-52%, then feeding the concentrated supernatant into a multistage vacuum flash crystallizer for flash continuous cooling crystallization, feeding crystallized crystal slurry into a slurry tank, separating the crystallized crystal slurry by a centrifuge to obtain a crystal grain material, washing impurities with purified water, then feeding the crystal grain material into a granulator for granulation, and drying the crystal grain material in a fluidized bed to obtain a finished product of the calcium gluconate.
Although the multistage continuous crystallization technology and equipment have advantages, the method has problems in the aspects of small product particle size, equipment scaling, easy flow blockage, short operation period and the like, and further research and improvement are needed. Therefore, a multifunctional crystallizer and a continuous crystallization method are needed, which not only can ensure the separation of crystal particles with different sizes, but also have wide application range and are suitable for large-scale popularization.
SUMMERY OF THE UTILITY MODEL
Not enough to prior art exists, the utility model aims to provide a multistage circulation crystallization system device, the utility model provides a multistage circulation crystallization system device not only can guarantee to realize the separation of variation in size crystallization granule, and application range is wide moreover, is fit for extensive the popularization.
To achieve the purpose, the utility model adopts the following technical proposal:
the utility model provides a multistage circulating crystallization system device, which comprises at least two circulating crystallization devices which are connected in series in sequence and have the same structure;
the circulating crystallization device comprises a shell, wherein a flow guide structure of a funnel structure is arranged in the shell, the flow guide structure comprises a flow guide conical section and a flow guide pipe section which are sequentially butted from top to bottom, and the edge of the large end face of the flow guide conical section is circumferentially butted with the inner wall of the shell;
a shell cavity above the flow guide conical section forms a mixing bin, a shell cavity at the periphery of the flow guide pipe section forms a crystallization bin, a stirring device is arranged at the bottom of an inner cavity of the shell, the outer wall of the mixing bin is provided with a feed inlet and at least one circulation inlet, the upper part of the outer wall of the crystallization bin is provided with at least one circulation outlet, the circulation inlet and the circulation outlet are communicated through an external circulation pipeline, the bottom of the outer wall of the crystallization bin is provided with a discharge port, and the discharge port is connected to a circulation pipeline of a next-stage circulation crystallization device or a feed inlet of the next-stage circulation crystallization device;
and the feed liquid is introduced into the mixing bin, mixed and enters the crystallization bin along the flow guide structure for crystallization, under the action of the stirring device, small-particle-size crystal grains form rotational flow in the crystallization bin and return to the mixing bin through the circulating pipeline for circulating crystallization, and large-particle-size crystal grains are settled and enter the next-stage circulating crystallization device through the discharge port for multistage continuous crystallization.
The utility model discloses establish ties a plurality of circulation crystallization device in proper order and can realize multistage continuous crystallization, be applicable to and be used for evaporative crystallization, solution crystallization, cooling crystallization and reaction crystallization, every level of crystallizer outside can be furnished with heating/cooling heat exchanger according to the crystallization mode, provides the heat/cold volume input that the crystallization process needs. In the multistage continuous crystallization process, the solid suspension amount of each stage of crystallization process needs to be controlled, taking a four-stage crystallization process as an example, the feeding material of the first stage circulating crystallization device is unsaturated crystallization material liquid or reaction liquid, the solid suspension amount in the first stage circulating crystallization device is controlled to be 2-10%, the solid suspension amount in the second stage circulating crystallization device is controlled to be 10-20%, the solid suspension amount in the third stage circulating crystallization device is controlled to be 20-30%, and the solid suspension amount in the fourth stage circulating crystallization device is controlled to be 30-45%. The utility model provides a multistage circulation crystal system device not only can guarantee to realize the separation of variation in size crystallization granule, and application range is wide moreover, is fit for extensive the popularization.
In addition, in order to guarantee that the crystalline grains fully grow in each level of crystallization process, the utility model discloses the inner structure to each level of circulation crystallization device has made the improvement equally, realized that the magma is at the inner loop and the particle size classification of single-stage crystallization process, in single-stage crystallization process, the magma can get into the crystallization bin along the structure of leaking hopper-shaped water conservancy diversion after getting into mixed storehouse, utilize the mobility of magma self, under the effect of agitating unit and crystalline grain self gravity, the crystalline grain of small particle size can move up and form certain circulation flow field in the crystallization bin under the wind-force effect of agitating unit, make the crystalline grain of small particle size suspend in the upper portion of crystallization bin, form the whirl circulation state, can not sink the end coalescence; and the crystal grains with large grain diameter can settle to the bottom of the crystallization bin, are discharged from the discharge port and enter the feed port of the next-stage crystallizer or are discharged as a final product, so that the grading treatment of the crystal grains is realized, and the grain diameter of the final product is improved. In addition, in the operation process, feed liquid containing small particles can be led out from a circulating outlet at the upper part of a crystallization bin, and the feed liquid has the characteristics of low crystal slurry density and small solid particle size, so that the problem that crystal particles with large particle size or large fallen scale deposits are easy to block when entering a pipeline is avoided.
As a preferable technical proposal of the utility model, a circulating pump is arranged on the circulating pipeline.
It should be noted that, the suspension in the crystallization bin sinks the crystal grains with large grain size due to the sedimentation, so the crystal grains with large grain size are mainly concentrated in the lower layer of the crystallization bin, the upper layer of the crystallization bin is suspension or clear liquid containing small grain size, the circulating pump pumps out the part of feed liquid from the circulating outlet and returns the part of feed liquid to the mixing bin, further crystallization grows, and the circulation is repeated until the crystal grains with ideal grain size are obtained.
And a conveying pump is arranged on a connecting pipeline between the discharge port of the circulating crystallization device and the circulating pipeline of the next-stage circulating crystallization device.
As an optimized technical scheme of the utility model, the last level the external aftertreatment system of discharge gate of circulation crystallization device.
As an optimized technical scheme of the utility model, be provided with mixing arrangement in the mixing bin, mixing arrangement includes at least two-layer stirring rake.
The utility model discloses in, mixing arrangement is preferred to include two-layer stirring rake, and the effect opposite direction of two-layer spiral stirring rake helps the dwell time of material in mixing the storehouse, guarantees the raw materials homogeneous mixing, and under the mechanical stirring effect, the feed liquid of the different temperatures of stranded and concentration is quick, abundant high-efficient mixing in the draft tube, and heat transfer, mass transfer are even, and the degree of supersaturation of feed liquid is even, avoids leading to the fact the outbreak nucleation because of local supersaturation is too high. It should be noted that, the function of the stirring paddle in the circulating crystallization device is to realize uniform mixing of the fluid, and the present invention does not make special requirements and specific limitations on the type and size of the stirring paddle, and those skilled in the art need to select the stirring paddle with a suitable size according to the size difference of the crystallization device.
Still be provided with spray set in the mixing bin, spray set's injection direction is just right mixing bin inner wall, spray set is used for to mixing bin inner wall sprays and dilutes the mother liquor.
The utility model discloses set up spray set on casing inner chamber upper portion, spray set can select to the annular shower, regularly sprays the dilution mother liquor to shells inner wall through spray set, can effectively erode the adnexed dirt layer of inner wall, and the inner wall scale deposit condition near crystallizer vapour-liquid boiling interface alleviates greatly, can not cause also that the bold dirt layer drops to pound bad crystallizer inner part or get into the situation emergence that extrinsic cycle heating/cooling heat exchanger blockked up the pipeline, has prolonged continuous production cycle.
As a preferred technical scheme, the outer wall in crystallization storehouse is including first conic section, drum section and the second conic section that from top to bottom docks in proper order, the little terminal surface of first conic section with mix the storehouse butt joint, the big terminal surface of first conic section with the one end butt joint of drum section, the other end of drum section with the big terminal surface butt joint of second conic section.
The outer edge of the large end face of the flow guide conical section is positioned at the butt joint of the first conical section and the mixing bin.
As an optimized technical scheme of the utility model, the outer wall department symmetry of mixing the storehouse is provided with at least two circulation entry, the outer wall department symmetry of first conic section is provided with at least two the circulation export, one the circulation export corresponds through independent circulation pipeline and connects one circulation entry.
The utility model is preferably provided with two circulation outlets and two circulation inlets, the circulation outlets are connected with the corresponding circulation inlets through independent circulation pipelines, and each circulation pipeline is provided with a circulation pump; the two circulating outlets are distributed in a symmetrical structure by using the central shaft of the crystallizing device, and the connecting line between the two circulating outlets is vertical to the direction of the stirring paddle.
The top of mixing the storehouse is provided with the feed inlet, the outer wall lower part of second cone section is provided with the discharge gate.
It should be noted that, in the crystallization process in which materials in different states are injected, the circulation inlet defined in the present invention can be used as a liquid inlet at the same time. In first order circulation crystallization device, the solid material can get into through the feed inlet at casing top, and the liquid material then gets into by circulation entry, and the feed liquor pipe can insert the casing alone, also can insert circulation line.
The material inflow mode of the circulating crystallization device at each stage is as follows: firstly, a discharge port of a previous stage of circulating crystallization device is connected with a circulating pipeline of a next stage of circulating crystallization device, and suspension (comprising large-particle-size crystal grains) discharged by the previous stage of circulating crystallization device is introduced into the circulating pipeline of the next stage of circulating crystallization device, mixed with crystal slurry circulated by the next stage of circulating crystallization device and then introduced into a mixing bin; and secondly, the suspension discharged from the discharge port of the previous stage of circulating crystallization device is connected to the feed port of the next stage of circulating crystallization device, the suspension (including large-grain-size crystal grains) discharged from the previous stage of circulating crystallization device is introduced into the mixing bin from the feed port of the next stage of circulating crystallization device, and the suspension discharged from the previous stage of circulating crystallization device and the crystal slurry circulated by the next stage of circulating crystallization device are mixed in the mixing bin.
As an optimal technical scheme of the utility model, the barrel diameter in mixed storehouse is less than the barrel diameter of drum section.
The height of the barrel body of the mixing bin is larger than or equal to the diameter of the barrel body of the mixing bin.
The height of the first conical section is smaller than that of the cylindrical section.
In a preferred embodiment of the present invention, the cylinder diameter of the mixing chamber is 0.6 to 0.8 times, for example, 0.6 times, 0.62 times, 0.64 times, 0.66 times, 0.68 times, 0.7 times, 0.72 times, 0.74 times, 0.76 times, 0.78 times, or 0.8 times the cylinder diameter of the cylinder section, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical value range are also applicable.
The barrel diameter of the mixing chamber is 1.2 to 3.5 times the barrel height of the mixing chamber, and may be, for example, 1.2 times, 1.4 times, 1.6 times, 1.8 times, 2.0 times, 2.2 times, 2.4 times, 2.6 times, 2.8 times, 3.0 times, 3.2 times, 3.4 times, or 3.5 times, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
The utility model discloses carried out special design to the partial size parameter among the circulation crystallization device, unique crystallizer configuration and flow operation, the product particle diameter that can improve continuous crystallization process is little, the scale deposit of crystallizer inner wall is serious, the pipeline blocks up, the problem that operating cycle is short etc.. The diameter of the cylinder of the mixing bin is specially limited to be 1.2-3.5 times of the height of the cylinder of the mixing bin, the diameter of the cylinder is increased, the evaporation area can be increased, the boiling strength of unit area is reduced, the splashing condition of materials is lightened, and the scaling of the materials on the inner wall of the crystallizer near a vapor-liquid interface caused by material entrainment caused by boiling of feed liquid in the evaporation crystallization process is reduced.
The height of the first conical section is 0.6 to 0.8 times the height of the cylindrical section, and may be, for example, 0.6, 0.62, 0.64, 0.66, 0.68, 0.7, 0.72, 0.74, 0.76, 0.78 or 0.8 times, but is not limited to the values recited, and other values not recited in this range of values are also applicable.
The diameter of the cylindrical section is 4 to 10 times, for example 4, 5, 6, 7, 8, 9 or 10 times, the diameter of the flow conduit section, but is not limited to the values listed and other values not listed in this range are equally applicable.
The length of the flow guide pipe section is 1/3-2/3 of the total height of the crystallization bin, and can be, for example, 0.35, 0.4, 0.45, 0.5, 0.55, 0.6 or 0.65, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
As an optimized technical scheme of the utility model, the water conservancy diversion conic section with the coaxial setting of water conservancy diversion pipeline section.
The diameter of the large end face of the flow guiding cone section is 4 to 10 times, for example 4, 5, 6, 7, 8, 9 or 10 times, the diameter of the flow guiding cone section is not limited to the values listed, and other values not listed in this range are also suitable.
As an optimized technical scheme of the utility model, the casing still include with the end storehouse of the little terminal surface butt joint of second cone section, agitating unit is located in the end storehouse.
The periphery of the stirring device is sleeved with a guide cylinder.
The utility model discloses establish the draft tube at agitating unit periphery cover for suspension in the crystallization bin downstream in the draft tube, the outer upward movement of draft tube realizes the magma homogeneous mixing.
The system refers to an equipment system, or a production equipment.
Illustratively, the circulation crystallizing device provided by the utility model is used for carrying out the crystallization reaction of baking soda, and the crystallization process specifically comprises the following steps:
(1) Under the condition of normal temperature, chemical fertilizer solid containing ammonium bicarbonate enters from a feed inlet at the top of a shell, liquid brine containing sodium chloride enters a mixing bin through a circulating inlet (a liquid inlet) along the tangential direction, mechanical stirring and mixing are carried out by a mixing device, the stirring speed is preferably 20-100 rpm, sodium chloride and ammonium bicarbonate in the brine are mixed and reacted to generate baking soda, and baking soda crystal slurry enters a crystallization bin downwards along a funnel-shaped flow guide structure under the action of the mixing device and the self gravity of the baking soda crystal slurry;
(2) After the crystal slurry enters a crystallizer bin, under the upward acting force of a bottom stirring device, the baking soda crystal slurry is upward along the inner wall of the crystallization bin, a circulation loop is formed at the periphery of a straight pipe section of a flow guide structure to reach a fluidized state, baking soda crystal grains with large particle size are settled under the action of gravity, baking soda crystal grains with small particle size are suspended on the upper layer of the crystallization bin, the automatic circulation of the crystal slurry in a crystallization bin body and the particle size classification of particles are realized, and finally, baking soda crystal grains with large particle size are gathered on the middle lower layer of the crystallization bin;
(3) The baking soda crystal grains with small grain sizes are returned to the mixing bin through a circulating pump through a circulating pipeline in the suspension process, at the moment, as the brine raw material is continuously introduced from a circulating inlet (liquid inlet), the baking soda crystal grains with small grain sizes which are circulated back are tangentially fed from the circulating inlet after being converged with new brine raw material, the process is repeated, and the baking soda crystal grains with small grain sizes are subjected to circulating crystal growth;
(4) And (3) collecting large-particle sodium bicarbonate grains to the bottom of the crystallization bin, discharging the large-particle sodium bicarbonate grains from a discharge port at the bottom, allowing the large-particle sodium bicarbonate grains to flow out of a suspension at the discharge port and enter a next-stage circulating crystallization device, similarly completing the operation steps of (1) to (4) in the next-stage circulating crystallization device, performing multi-stage continuous crystallization, and performing evaporative crystallization, solventing-out crystallization, cooling crystallization or reaction crystallization to complete a multi-stage continuous crystallization process, wherein a discharge material liquid of a last-stage circulating crystallization device enters solid-liquid separation equipment, and a grain product is obtained after solid-liquid separation.
It should be noted that the present invention provides a multistage circulation crystallization system device suitable for multistage crystallization operations such as evaporative crystallization, elution crystallization, cooling crystallization or reactive crystallization, but the specific operating process conditions need to be adjusted by those skilled in the art based on different crystallization modes, and the present invention does not require and is not limited to the following specific requirements and limitations, for example: the operating pressure and temperature of each stage of crystallizer for reduced pressure evaporation crystallization are gradually reduced, and the reaction crystallization/elution crystallization is gradually increased by adding reaction materials or elution agent materials into each stage of circulating crystallization device. In addition, the number of stages of the circulating crystallization device is determined by the solid content in the crystal slurry, and the solid content and the grain diameter of crystal grains in the final circulating crystallization device are maximum.
Compared with the prior art, the beneficial effects of the utility model are that:
(1) The utility model discloses establish ties a plurality of circulation crystallization device in proper order and can realize multistage continuous crystallization, be applicable to and be used for evaporative crystallization, dissolve out crystallization, cooling crystallization and reaction crystallization, every grade of crystallizer outside can be furnished with heating/cooling heat exchanger according to the crystallization mode, provides the heat/cold volume input that the crystallization process needs. In the multistage continuous crystallization process, the solid suspension amount of each stage of crystallization process needs to be controlled, taking a four-stage crystallization process as an example, the feeding material of the first stage circulating crystallization device is unsaturated crystallization material liquid or reaction liquid, the solid suspension amount in the first stage circulating crystallization device is controlled to be 2-10%, the solid suspension amount in the second stage circulating crystallization device is controlled to be 10-20%, the solid suspension amount in the third stage circulating crystallization device is controlled to be 20-30%, and the solid suspension amount in the fourth stage circulating crystallization device is controlled to be 30-45%. The utility model provides a multistage circulation crystal system device not only can guarantee to realize the separation of variation in size crystallization granule, and application range is wide moreover, is fit for extensive the popularization.
(2) In order to guarantee that crystalline grains fully grow in each stage of crystallization process, the utility model discloses the inner structure to each stage of circulation crystallization device has made the improvement equally, realized that the magma is at the inner loop and the particle size of single-stage crystallization process hierarchical, in single-stage crystallization process, the magma can get into the crystallization bin along the water conservancy diversion structure of leaking hopper-shaped after getting into mixed storehouse, utilize the mobility of magma self, under the effect of agitating unit and crystalline grain self gravity, the crystalline grain of small particle size can move up and form certain circulation flow field in the crystallization bin under agitating unit's wind-force effect, make the crystalline grain of small particle size suspend in the upper portion in crystallization bin, form whirl circulation state, can not sink the end coalescence; and the crystal grains with large grain diameter can settle to the bottom of the crystallization bin, are discharged from the discharge port and enter the feed port of the next-stage crystallizer or are discharged as a final product, so that the grading treatment of the crystal grains is realized, and the grain diameter of the final product is improved. In addition, in the operation process, feed liquid containing small particles can be led out from a circulating outlet at the upper part of a crystallization bin, and the feed liquid has the characteristics of low crystal slurry density and small solid particle size, so that the problem that crystal particles with large particle size or large fallen scale deposits are easy to block when entering a pipeline is avoided.
Drawings
Fig. 1 is a schematic structural diagram of a two-stage circulation crystallization system apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a four-stage circulating crystallization system apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a circulating crystallization apparatus according to an embodiment of the present invention;
wherein, 1-a feed inlet; 2-a mixing device; 3-a first recycle inlet; 4-a first recycle outlet; 5-discharging port; 6-a stirring device; 7-a second recycle inlet; 8-a mixing bin; 9-a second recycle outlet; 10-a crystallization bin; 11-a flow guide structure; 12-a guide shell; 13-bottom bin; 14-a cyclic crystallization device; 15-a circulation pump; 16-delivery pump.
Detailed Description
It is to be understood that in the description of the present invention, the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for the purpose of convenience and simplicity of description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
It should be noted that, unless explicitly stated or limited otherwise, the terms "disposed," "connected" and "connected" in the description of the present invention are to be construed broadly, and may for example be fixedly connected, detachably connected or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
It should be understood that the present invention includes the necessary pipeline, conventional valve and general pump equipment for realizing the complete process, but the above contents do not belong to the main innovation point of the present invention, and the skilled person can select the type based on the process flow and the equipment structure to add the layout by himself, and the present invention does not have the special requirement and limitation.
The technical solution of the present invention is further explained by the following embodiments with reference to the accompanying drawings.
In one embodiment, the present invention provides a multistage circulating crystallization system apparatus, as shown in fig. 1 and 2, comprising at least two structurally identical circulating crystallization apparatuses 14 connected in series in sequence;
as shown in fig. 3, the circulating crystallization device 14 includes a housing, a flow guide structure 11 of a funnel structure is disposed in the housing, the flow guide structure 11 includes a flow guide conical section and a flow guide pipe section which are sequentially butted from top to bottom, and the edge of the large end surface of the flow guide conical section is butted with the inner wall of the housing in the circumferential direction;
a shell cavity above the flow guide conical section forms a mixing bin 8, a shell cavity at the periphery of the flow guide pipe section forms a crystallization bin 10, a stirring device 6 is arranged at the bottom of an inner cavity of the shell, a feed inlet 1 and at least one circulation inlet are formed in the outer wall of the mixing bin 8, at least one circulation outlet is formed in the upper portion of the outer wall of the crystallization bin 10, the circulation inlet is communicated with the circulation outlet through an external circulation pipeline, a discharge outlet 5 is formed in the bottom of the outer wall of the crystallization bin 10, and the discharge outlet 5 is connected to a circulation pipeline of a next-stage circulation crystallizing device 14 or the feed inlet 1 of the next-stage circulation crystallizing device 14;
and the feed liquid is introduced into the mixing bin 8, mixed and enters the crystallization bin 10 along the flow guide structure 11 for crystallization, small grain size crystal grains form rotational flow in the crystallization bin 10 under the action of the stirring device 6 and return to the mixing bin 8 through the circulation pipeline for circulation crystallization, and large grain size crystal grains are settled and enter the next stage of circulation crystallization device 14 through the discharge port 5 for multistage continuous crystallization.
The utility model discloses establish ties a plurality of circulation crystallization device 14 in proper order and can realize multistage continuous crystallization, be applicable to and be used for the evaporative crystallization, dissolve out crystallization, cooling crystallization and reaction crystallization, every level of crystallizer outside can be furnished with heating/cooling heat exchanger according to the crystallization mode, provides the heat/cold volume input that the crystallization process needs. In the multistage continuous crystallization process, the solid suspension amount of each stage of crystallization process needs to be controlled, taking a four-stage crystallization process as an example, the feeding material of the first stage circulating crystallization device 14 is unsaturated crystallization material liquid or reaction liquid, the solid suspension amount in the first stage circulating crystallization device 14 is controlled to be 2% -10%, the solid suspension amount in the second stage circulating crystallization device 14 is controlled to be 10% -20%, the solid suspension amount in the third stage circulating crystallization device 14 is controlled to be 20% -30%, and the solid suspension amount in the fourth stage circulating crystallization device 14 is controlled to be 30% -45%. The utility model provides a multistage circulation crystal system device not only can guarantee to realize the separation of variation in size crystallization granule, and application range is wide moreover, is fit for extensive the popularization.
In addition, in order to guarantee that the crystalline grains fully grow in each level of crystallization process, the utility model discloses the inner structure to each level of circulation crystallization device 14 has made the improvement equally, realized that the magma is at the inner loop and the particle size classification of single-stage crystallization process, in single-stage crystallization process, the magma can get into crystallization bin 10 along leaking hopper-shaped water conservancy diversion structure 11 after getting into mixing storehouse 8, utilize the mobility of magma self, under the effect of agitating unit 6 and crystalline grain self gravity, the crystalline grain of small particle size can upwards move and form certain circulation flow field in crystallization bin 10 under the wind-force effect of agitating unit 6, make the crystalline grain of small particle size suspend in the upper portion of crystallization bin 10, form whirl circulation state, can not sink the end coalescence; and the crystal grains with large grain diameter can settle to the bottom of the crystallization bin 10, are discharged from the discharge port 5, enter the feed port 1 of the next-stage crystallizer or are discharged as final products, thereby realizing the grading treatment of the crystal grains and improving the grain diameter of the final products. In addition, in the operation process, feed liquid containing small particles can be led out from a circulating outlet at the upper part of the crystallization bin 10, and the feed liquid has the characteristics of low crystal slurry density and small solid particle size, so that the problem that crystal particles with large particle size or large fallen scale deposits enter a pipeline and are easy to block is avoided.
Further, a circulation pump 15 is provided on the circulation line.
It should be noted that, the suspension in the crystallization bin 10 sinks the crystal grains with large grain size due to the sedimentation effect, so the crystal grains with large grain size are mainly concentrated in the lower layer of the crystallization bin 10, the suspension or clear liquid with small grain size is arranged in the upper layer of the crystallization bin 10, the circulating pump 15 pumps out the part of the feed liquid from the circulating outlet and returns the part of the feed liquid to the mixing bin 8, further crystallization grows, and the circulation is repeated until the crystal grains with ideal grain size are obtained.
A delivery pump 16 is arranged on a connecting pipeline between the discharge port 5 of the circulating crystallization device 14 and the circulating pipeline of the next-stage circulating crystallization device 14.
Further, the discharge port 5 of the last stage of the circulating crystallization device 14 is externally connected with an after-treatment system.
Further, a mixing device 2 is arranged in the mixing bin 8, and the mixing device 2 comprises at least two layers of stirring paddles.
The utility model discloses in, 2 preferred including two-layer stirring rake of mixing arrangement, the effect opposite direction of two-layer spiral stirring rake helps the dwell time of material in mixing bin 8, guarantees the raw materials homogeneous mixing, under the mechanical stirring effect, the feed liquid of stranded different temperatures and concentration is quick, abundant high-efficient mixing in draft tube 12, and heat transfer, mass transfer are even, and the degree of supersaturation of feed liquid is even, avoids leading to the fact the outbreak nucleation because of local supersaturation is too high. It should be noted that the function of the stirring paddle in the circulating crystallization device 14 is to achieve uniform mixing of the fluid, and the present invention does not make special requirements and specific limitations on the type and size of the stirring paddle, and those skilled in the art need to select the stirring paddle with a suitable size according to the size difference of the crystallization device.
Still be provided with spray set in the mixing bin 8, spray set's injection direction is just right mixing bin 8 inner wall, spray set is used for to 8 inner walls in mixing bin spray dilution mother liquor.
The utility model discloses set up spray set on casing inner chamber upper portion, spray set can select to the annular shower, regularly sprays the dilution mother liquor to shells inner wall through spray set, can effectively erode the adnexed dirt layer of inner wall, and the inner wall scale deposit condition near crystallizer vapour-liquid boiling interface alleviates greatly, can not cause also that the bold dirt layer drops to pound bad crystallizer inner part or get into the situation emergence that extrinsic cycle heating/cooling heat exchanger blockked up the pipeline, has prolonged continuous production cycle.
Further, the outer wall of crystallization storehouse 10 is including first conic section, drum section and the second conic section of butt joint from top to bottom in proper order, the little terminal surface of first conic section with mix 8 butt joints in the storehouse, the big terminal surface of first conic section with the one end butt joint of drum section, the other end of drum section with the big terminal surface butt joint of second conic section.
The outer edge of the large end face of the flow guide conical section is positioned at the butt joint of the first conical section and the mixing bin 8.
Furthermore, the outer wall of the mixing bin 8 is symmetrically provided with at least two circulation inlets, the outer wall of the first conical section is symmetrically provided with at least two circulation outlets, and one circulation outlet is correspondingly connected with one circulation inlet through an independent circulation pipeline.
The utility model is preferably provided with two circulation outlets (as shown in figure 1, a first circulation outlet 4 and a second circulation outlet 9) and two circulation inlets (as shown in figure 1, a first circulation inlet 3 and a second circulation inlet 7), wherein the circulation outlets are connected with the corresponding circulation inlets through independent circulation pipelines, and each circulation pipeline is provided with a circulation pump 15; the two circulating outlets are distributed in a symmetrical structure by using the central shaft of the crystallizing device, and the connecting line between the two circulating outlets is vertical to the direction of the stirring paddle.
The top of mixing bin 8 is provided with feed inlet 1, the outer wall lower part of second cone section is provided with discharge gate 5.
It should be noted that, in the crystallization process in which materials in different states need to be injected, the circulation inlet defined in the present invention can be used as a liquid inlet at the same time. In the first-stage circulating crystallization device 14, solid materials can enter through a feed inlet 1 at the top of the shell, liquid materials enter through a circulating inlet, and a liquid inlet pipe can be independently connected into the shell and also can be connected into a circulating pipeline.
The material inflow mode of the circulating crystallizing devices 14 at each stage is divided into two modes: firstly, a discharge port 5 of a previous stage of circulating crystallization device 14 is connected with a circulating pipeline of a next stage of circulating crystallization device 14, and suspension (including large-particle-size crystal grains) discharged from the previous stage of circulating crystallization device 14 is introduced into the circulating pipeline of the next stage of circulating crystallization device 14, mixed with crystal slurry circulated by the next stage of circulating crystallization device 14 and then introduced into a mixing bin 8; secondly, the suspension discharged from the discharge port 5 of the previous stage of the circulating crystallization device 14 is connected to the feed port 1 of the next stage of the circulating crystallization device 14, the suspension (including large grain size crystal grains) discharged from the previous stage of the circulating crystallization device 14 is introduced into the mixing bin 8 from the feed port 1 of the next stage of the circulating crystallization device 14, and the suspension discharged from the previous stage of the circulating crystallization device 14 is mixed with the crystal slurry circulated by the next stage of the circulating crystallization device 14 in the mixing bin 8.
Further, the cylinder diameter of the mixing bin 8 is smaller than the cylinder diameter of the cylinder section.
The height of the cylinder body of the mixing bin 8 is more than or equal to the diameter of the cylinder body of the mixing bin 8.
The height of the first conical section is smaller than that of the cylindrical section.
Further, the diameter of the cylinder of the mixing bin 8 is 0.6-0.8 times of the diameter of the cylinder section. The diameter of the cylinder body of the mixing bin 8 is 1.2-3.5 times of the height of the cylinder body of the mixing bin 8.
The utility model discloses carried out special design to the partial size parameter among the circulation crystallization device 14, unique crystallizer configuration and flow operation, the product particle diameter that can improve continuous crystallization process is little, the crystallizer inner wall scale deposit is serious, the pipeline blocks up, the problem that operating cycle is short etc.. The diameter of the mixing bin 8 is specially limited to be 1.2-3.5 times of the height of the mixing bin 8, the diameter of the mixing bin is increased, the evaporation area can be increased, the boiling strength of a unit area is reduced, the splashing condition of materials is relieved, and the scaling of the materials on the inner wall of the crystallizer near a vapor-liquid interface caused by the entrainment of the materials due to the boiling of feed liquid in the evaporation crystallization process is reduced.
The height of the first conical section is 0.6-0.8 times of the height of the cylindrical section. The diameter of the cylinder section is 4-10 times of that of the diversion pipe section. The length of the flow guide pipe section is 1/3-2/3 of the total height of the crystallization bin 10.
Furthermore, the flow guide conical section and the flow guide pipe section are coaxially arranged. The diameter of the large end surface of the flow guide conical section is 4-10 times of the diameter of the flow guide pipe section.
Further, the shell further comprises a bottom bin 13 butted with the small end face of the second conical section, and the stirring device 6 is positioned in the bottom bin 13.
The periphery of the stirring device 6 is sleeved with a guide shell 12.
The utility model discloses draft tube 12 is established to 6 periphery covers at agitating unit for the suspension in crystallization storehouse 10 downstream in draft tube 12, the outside upward movement of draft tube 12 realizes the magma homogeneous mixing.
In another embodiment, the present invention provides a circulation crystallizing device 14 for crystallizing baking soda, wherein the crystallization process specifically comprises the following steps:
(1) Under the condition of normal temperature, chemical fertilizer solid containing ammonium bicarbonate enters from a feed inlet 1 at the top of a shell, liquid brine containing sodium chloride enters a mixing bin 8 through a circulating inlet (a liquid inlet) along the tangential direction, the brine is mechanically stirred and mixed by a mixing device 2, the stirring speed is preferably 20-100 rpm, sodium chloride and ammonium bicarbonate in the brine are mixed and reacted to generate baking soda, and baking soda crystal slurry enters a crystallization bin 10 downwards along a funnel-shaped flow guide structure 11 under the action of the mixing device 2 and the gravity of the mixing device;
(2) After the crystal slurry enters a crystallizer bin, under the upward acting force of a bottom stirring device 6, the baking soda crystal slurry is upward along the inner wall of the crystallization bin 10, a circulation loop is formed at the periphery of a straight pipe section of a flow guide structure 11 to reach a fluidized state, baking soda crystal grains with large grain diameters are settled under the action of gravity, baking soda crystal grains with small grain diameters are suspended on the upper layer of the crystallization bin 10, the automatic circulation of the crystal slurry in the crystallization bin 10 and the grain diameter grading of grains are realized, and finally, baking soda crystal grains with large grain diameters are gathered on the middle-lower layer of the crystallization bin 10;
(3) The baking soda grains with small grain size are returned to the mixing bin 8 through a circulating pipeline by a circulating pump 15 in the suspension process, at the moment, the baking soda grains with small grain size which are circulated back are tangentially fed from a circulating inlet after being converged with a new brine raw material along with the continuous introduction of the brine raw material from the circulating inlet (liquid inlet), and the process is repeated to carry out circulating crystallization growth on the baking soda grains with small grain size;
(4) Collecting large-particle baking soda grains to the bottom of a crystallization bin 10, discharging the large-particle baking soda grains from a discharge port 5 at the bottom, allowing the large-particle baking soda grains to flow out from the discharge port 5 along with suspension liquid to enter a next-stage circulating crystallization device 14, similarly completing the operation steps of (1) to (4) in the next-stage circulating crystallization device 14, performing multi-stage continuous crystallization, evaporative crystallization, solventing-out crystallization, cooling crystallization or reaction crystallization, completing a multi-stage continuous crystallization process, allowing a discharge material liquid of a last-stage circulating crystallization device 14 to enter solid-liquid separation equipment, and performing solid-liquid separation to obtain a grain product.
It should be noted that the present invention provides a multistage circulation crystallization system device suitable for multistage crystallization operations such as evaporative crystallization, elution crystallization, cooling crystallization or reactive crystallization, but the specific operating process conditions need to be adjusted by those skilled in the art based on different crystallization modes, and the present invention does not require and is not limited to the following specific requirements and limitations, for example: the operating pressure and temperature of each stage of crystallizer for reduced pressure evaporation crystallization are gradually reduced, and the reaction crystallization/elution crystallization is gradually increased by adding reaction materials or elution agent materials into each stage of circulating crystallization device 14. In addition, the number of stages of the circulating crystallizing device 14 is determined by the solid content in the crystal slurry, and the solid content and the grain diameter of the crystal grains in the final stage circulating crystallizing device 14 are the largest.
The applicant states that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and those skilled in the art should understand that any changes or substitutions easily conceivable by those skilled in the art within the technical scope of the present invention are within the protection scope and the disclosure scope of the present invention.
Claims (10)
1. The multistage circulating crystallization system device is characterized by comprising at least two circulating crystallization devices which are sequentially connected in series and have the same structure;
the circulating crystallization device comprises a shell, wherein a flow guide structure of a funnel structure is arranged in the shell, the flow guide structure comprises a flow guide conical section and a flow guide pipe section which are sequentially butted from top to bottom, and the edge of the large end face of the flow guide conical section is circumferentially butted with the inner wall of the shell;
a shell cavity above the flow guide conical section forms a mixing bin, a shell cavity at the periphery of the flow guide pipe section forms a crystallization bin, a stirring device is arranged at the bottom of an inner cavity of the shell, a feed inlet and at least one circulation inlet are formed in the outer wall of the mixing bin, at least one circulation outlet is formed in the upper part of the outer wall of the crystallization bin, the circulation inlet is communicated with the circulation outlet through an external circulation pipeline, a discharge outlet is formed in the bottom of the outer wall of the crystallization bin, and the discharge outlet is connected to a circulation pipeline of a next-stage circulation crystallization device or a feed inlet of the next-stage circulation crystallization device;
and the feed liquid is introduced into the mixing bin, mixed and enters the crystallization bin along the flow guide structure for crystallization, under the action of the stirring device, small-particle-size crystal grains form rotational flow in the crystallization bin and return to the mixing bin through the circulating pipeline for circulating crystallization, and large-particle-size crystal grains are settled and then enter the next-stage circulating crystallization device through the discharge port for multistage continuous crystallization.
2. The multi-stage circulation crystallization system apparatus according to claim 1, wherein a circulation pump is provided on the circulation line;
and a conveying pump is arranged on a connecting pipeline between the discharge port of the circulating crystallization device and the circulating pipeline of the next-stage circulating crystallization device.
3. The multi-stage circulating crystallization system device of claim 2, wherein the discharge port of the last stage of circulating crystallization device is externally connected with an after-treatment system.
4. The multistage circulating crystallization system device of claim 1, wherein a mixing device is disposed in the mixing bin, the mixing device comprising at least two layers of stirring paddles;
still be provided with spray set in the mixing bin, spray set's injection direction is just right mixing bin inner wall, spray set is used for to mixing bin inner wall sprays and dilutes the mother liquor.
5. The multistage circulation crystallization system device of claim 1, wherein the outer wall of the crystallization bin comprises a first conical section, a cylindrical section and a second conical section which are sequentially butted from top to bottom, the small end surface of the first conical section is butted with the mixing bin, the large end surface of the first conical section is butted with one end of the cylindrical section, and the other end of the cylindrical section is butted with the large end surface of the second conical section;
the outer edge of the large end face of the flow guide conical section is positioned at the butt joint of the first conical section and the mixing bin.
6. The multistage circulation crystallization system device of claim 5, wherein at least two circulation inlets are symmetrically arranged on the outer wall of the mixing bin, at least two circulation outlets are symmetrically arranged on the outer wall of the first conical section, and one circulation outlet is correspondingly connected with one circulation inlet through an independent circulation pipeline;
the top of mixing the storehouse is provided with the feed inlet, the outer wall lower part of second cone section is provided with the discharge gate.
7. The multi-stage circulating crystallization system apparatus of claim 5, wherein the barrel diameter of the mixing bin is smaller than the barrel diameter of the barrel section;
the height of the cylinder body of the mixing bin is more than or equal to the diameter of the cylinder body of the mixing bin;
the height of the first conical section is smaller than that of the cylindrical section.
8. The multistage circulating crystallization system device of claim 7, wherein the cylinder diameter of the mixing bin is 0.6 to 0.8 times the cylinder diameter of the cylinder section;
the diameter of the cylinder body of the mixing bin is 1.2-3.5 times of the height of the cylinder body of the mixing bin;
the height of the first conical section is 0.6 to 0.8 time of the height of the cylindrical section;
the diameter of the cylinder section is 4-10 times of that of the diversion pipe section;
the length of the flow guide pipe section is 1/3-2/3 of the total height of the crystallization bin.
9. The multi-stage circulating crystallization system apparatus of claim 1, wherein the flow guiding cone section is coaxially arranged with the flow guiding pipe section;
the diameter of the large end surface of the flow guide conical section is 4-10 times of the diameter of the flow guide pipe section.
10. The multi-stage circulating crystallization system apparatus of claim 5, wherein the housing further comprises a bottom bin abutting against the small end face of the second conical section, the stirring device being located within the bottom bin;
the periphery of the stirring device is sleeved with a guide cylinder.
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| CN202221189770.1U CN217887033U (en) | 2022-05-18 | 2022-05-18 | Multistage circulation crystallization system device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202221189770.1U CN217887033U (en) | 2022-05-18 | 2022-05-18 | Multistage circulation crystallization system device |
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