WO2020019542A1 - Vertical vacuum crystallizing apparatus - Google Patents

Vertical vacuum crystallizing apparatus Download PDF

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Publication number
WO2020019542A1
WO2020019542A1 PCT/CN2018/111214 CN2018111214W WO2020019542A1 WO 2020019542 A1 WO2020019542 A1 WO 2020019542A1 CN 2018111214 W CN2018111214 W CN 2018111214W WO 2020019542 A1 WO2020019542 A1 WO 2020019542A1
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liquid
cylinder
condensing
section
vertical vacuum
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PCT/CN2018/111214
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French (fr)
Chinese (zh)
Inventor
陈爱民
沈梅和
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江苏新宏大集团有限公司
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Publication of WO2020019542A1 publication Critical patent/WO2020019542A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0018—Evaporation of components of the mixture to be separated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets

Definitions

  • the invention relates to the field of chemical separation, in particular to a vertical vacuum crystallization device.
  • Crystallization refers to the process by which solids are precipitated from gases, liquids or melts in a crystalline state. This process is determined by thermodynamic and kinetic factors. To solute from a solution, energy must be continuously obtained from the outside to make the solution in the solution constantly Evaporate to make it saturated and supersaturated. When the solution is not saturated (in the stable region), the solute will not crystallize. When the solution is between the solubility curve and the supersolubility curve (metastatic region), the solute crystals and The dissolution is in a dynamic equilibrium, solutes will not spontaneously nucleate and precipitate. If crystal nuclei enter, crystals can grow out.
  • This stage is extremely susceptible to external influences, such as the presence or absence of seeds, the size of seeds, the number of seeds, the presence of stirring, vibration and Factors such as impurities, crystal growth should be controlled within this region.
  • crystal growth should be controlled within this region.
  • the formation of crystal nuclei can be divided into two types: primary nucleation without crystals and secondary nucleation with crystals.
  • secondary nucleation is usually controlled, that is, shear stress nucleation and contact nucleation of fluids. That is to choose the appropriate stirring type and speed.
  • the driving force for crystal growth is the supersaturation concentration difference and the transmission speed of the solution.
  • the solute in the supersaturated solution diffuses into the relatively stationary liquid layer near the crystal nuclei, and passes through the relatively stationary solution layer to the crystal surface to embed the crystal plane.
  • the crystal grows up and releases the heat of crystallization. The heat is then transferred to the solution by diffusion.
  • the circulating solution flow rate is the same when the evaporation amount is constant.
  • the circulating solution flow rate and the solution's supersaturation are inversely proportional to each other, and the circulating flow rate determines the flow velocity of the various parts of the evaporation crystallizer.
  • the collision between the crystal and the wall of the device is intensified, which increases the possibility of the crystal breaking into secondary crystal nuclei and has a great impact on the particle size of the product.
  • the small flow rate is not conducive to the growth of the crystal, so an appropriate circulation flow rate is required. .
  • Crystal slurry concentration Under other conditions, if the concentration of the crystal slurry is high, the crystal retention in the crystallizer will increase, and the crystal residence time will increase, which is beneficial to the elimination of solution supersaturation and crystal growth. If it is too high, the chance of collision between crystals, between the crystal and the wall will increase, and the probability of crystals being broken into secondary crystal nuclei will increase, which is also detrimental to crystal growth. Therefore, the appropriate crystal concentration should be controlled. Generally, the solid-liquid ratio is controlled at 20%.
  • the most commonly used crystallization method is to use forced external circulation.
  • the feed liquid is added from the lower part of the circulation tube, mixed with the crystal slurry leaving the bottom of the crystallization chamber, and then pumped to the heating chamber.
  • the crystal slurry is heated in a heating chamber (usually 2 to 6 ° C), but evaporation does not occur.
  • the hot crystal slurry boils after entering the crystallization chamber, so that the solution reaches a supersaturated state, so part of the solute is deposited on the surface of the suspended grains, and the crystal grows.
  • the crystal slurry as a product is discharged from the upper part of the circulation pipe.
  • the forced circulation evaporation crystallizer has a large production capacity, but because there is no stirring device in the crystallizer, the mixing degree of the slurry becomes poor, resulting in a wide particle size distribution of the product; and because of the external circulation cooling in the device, its cooling pipe Will be easier to scale.
  • the present invention proposes a vertical vacuum crystallization device.
  • a vertical vacuum crystallization device which is characterized by comprising: a crystallization part and a condensation part;
  • the crystallization part includes a crystallization section cylinder, an outer deflector, a central deflector, a bottom stirrer, a secondary steam rising cylinder, a circulation pump, an inner circulation channel and an outer circulation channel;
  • the crystallization section cylinder is an axisymmetric structure with a central axis, and includes a frustum-shaped upper part, a straight middle part, and a tapered bottom connected in sequence.
  • the straight middle part includes an upper end and a lower end, and a large round bottom surface of the frustum-shaped upper part and The upper end is connected, the bottom surface of the tapered bottom is connected to the lower end, a clear solution outlet is provided at the middle position of the straight cylindrical middle, and the central axis is a symmetrical axis on the tapered bottom, symmetrically There are inlet and outlet openings;
  • the outer diversion cylinder includes first and second opposite ends, the outer diversion cylinder is located inside the crystallization section cylinder, and the first end is fixedly connected to the straight middle portion through a diameter reduction. The intersection of the reduced diameter and the straight middle portion is located above the outlet of the clear solution, the second end is on the same horizontal line as the lower end of the straight middle portion, and the outer diversion tube is based on the Central axis axisymmetric;
  • the central baffle includes a third end and a fourth end opposite to each other.
  • the central baffle is located inside the outer baffle, and a horizontal level at which the third end is located is higher than the outer baffle.
  • the liquid surface at the upper part of the third end is an evaporation interface
  • the height of the fourth end at the horizontal plane is lower than the height of the second end at the horizontal plane, and the central guide tube Axisymmetric about the central axis;
  • the bottom stirrer is located inside the fourth end;
  • the secondary steam rising cylinder has a cylindrical structure and is connected to the top end of the frustum-shaped upper part and is axially symmetrical with the central axis;
  • the circulation pump is located outside the barrel of the crystallization section, and is connected to the feed inlet and the clear solution outlet through a pipeline;
  • the inner circulation channel of the central deflector and the channel between the outer deflector and the central deflector form the inner circulation channel
  • a passage between the outer deflector and the cylindrical middle portion is a clarification zone, and the inner circulation passage, the clarification zone, the circulation pump, and the pipeline form the outer circulation passage;
  • the condensing section includes a condensing section cylinder and an overflow weir, a first water-retaining cap, a liquid folding ring and a second water-retaining cap which are sequentially arranged from the top to the bottom of the condensing-section cylinder.
  • the overflow weir, the first water-retaining cap, the liquid-retaining ring, and the second water-retaining cap are all symmetrical about the central axis, and the condensation part is located above the crystal part
  • the bottom end of the condensing section cylinder covers the second steam rising cylinder and is fixedly connected to the outer side of the frustum-shaped upper part.
  • the lower edge of the overflow weir is sealedly connected to the condensing section cylinder.
  • the overflow weir The diameter of the upper edge is less than or equal to the water-retaining width of the first water-retaining cap.
  • the liquid-retaining ring is located between the first and second water-retaining caps.
  • the edge is fixed on the cylinder of the condensation section, and the inner diameter of the liquid-retaining ring is less than or equal to the width of the first water retaining cap and less than or equal to the width of the second water retaining cap.
  • the segment cylinder is provided with a cooling liquid injection port at the position of the overflow weir.
  • the bottom stirrer is a push-type stirrer, which is used to push the mixed solution in the central draft tube to the evaporation interface on the upper part of the central draft tube to make the inner circulation efficiency in the inner circulation channel. improve.
  • an upper part of the condensing section cylinder is provided with a non-condensable gas outlet, and the non-condensable gas outlet is located above the overflow weir to discharge the non-condensable gas in the secondary steam from the condensation. Segment tube.
  • the pipeline outside the outlet of the clarification solution is connected to a fine crystal water pipe, which is used to mix the fine crystal water with the crystallization solution to eliminate fine crystals in the crystallization solution.
  • a cooling condensate mixed liquid inlet is provided at the lower part of the barrel of the condensation section, and the height of the cooling condensate mixed liquid outlet from the ground is less than the height of the secondary steam rising tube from the ground.
  • the condensing part further includes a liquid-sealing tank and an atmospheric leg, one end of the atmospheric leg is connected to the cooling and condensing mixed liquid outlet, and the other end of the atmospheric leg is connected to the liquid-sealing tank for
  • the cooled and condensed mixed liquid in the condensing section cylinder was successfully drawn out into the liquid-sealed tank.
  • the atmospheric leg was filled with liquid and the height of the liquid column in the atmospheric leg was between 10 and 20 meters. So that the cooling and condensing mixed liquid automatically enters the liquid-sealing tank by the gravity of the liquid column.
  • a cooling liquid de-heating port is provided at the bottom of the liquid sealing tank, and the cooling liquid de-heating port is connected to the cooling liquid injection port through a circulation pipe.
  • the diameter of the outer diversion cylinder is twice the diameter of the central diversion cylinder to provide sufficient space for the outer circulation channel to eliminate excessive fine crystals and the granularity of the elutriation product.
  • the crystallizing section further includes a product slurry pump, and the product slurry pump is connected to the discharge port through a pipe, and is used for drawing out the crystals generated by the crystallizing section.
  • the vertical vacuum crystallization device is a multi-stage series structure, and the outlet end of the circulation pump of one of the two adjacent vertical vacuum crystallization devices is simultaneously with the other of the two adjacent vertical vacuum crystallization devices.
  • the inlet of one is connected.
  • the main equipment of a vertical vacuum crystallization device of the present invention is simple, does not require a heat exchanger, does not have serious scaling on the inner surface, and does not have scaling cleaning problems, thereby affecting production capacity; the vacuum operating pressure and The partial vapor pressure of the solution is similar, and the operation is relatively stable.
  • the crystallization section and the condensation section are combined into one device, which is different from other forms of crystallization evaporator and condenser. Its main advantage is that it does not need to use pipes to introduce the secondary steam from the crystallization section to the condensation section, which shortens the secondary steam flow.
  • the temperature increases the evaporation of the solution, saves power consumption, and saves equipment investment.
  • the internal circulation channel of the invention eliminates the high saturation area in the crystallizer, and the saturation in the crystallizer is relatively uniform and low, which improves the evaporation intensity, strengthens the production capacity of the crystallizer, and promotes the application of the agitator to improve Internal circulation efficiency reduces the chance of nucleation and fragmentation when crystals and blades collide.
  • the mixer uses variable frequency speed regulation to help adjust the production load; the external circulation channel eliminates excessive fine crystals and the elutriation of product size to ensure Produces products with a narrow particle size distribution.
  • FIG. 1 is a schematic diagram of the overall structure of a vertical vacuum crystallization apparatus of the present invention.
  • FIG. 1 is a schematic diagram of an overall structure of a vertical vacuum crystallization apparatus according to the present invention.
  • a vertical vacuum crystallization apparatus according to an embodiment of the present invention includes a crystallization section 1 and a condensation section 2.
  • the crystallization section 1 includes a crystallization section cylinder 3, an outer deflector 4, a center deflector 5, a bottom stirrer 6, a secondary steam riser 7, a circulation pump 8, an inner circulation channel, and an outer circulation channel.
  • the crystalline section cylinder 3 is an axisymmetric structure with a central axis 31, and includes a frustum-shaped upper portion 32, a straight cylindrical middle portion 33, and a tapered bottom portion 34 connected in sequence.
  • the straight cylindrical middle portion 33 includes an upper end 331 and a lower end 332, and the frustum-shaped upper portion 32
  • the large round bottom surface is connected to the upper end 331, the bottom surface of the tapered bottom portion 34 is connected to the lower end 332, a clear solution outlet 35 is provided in the middle of the straight cylindrical middle portion 33
  • the central axis 31 is a symmetrical axis on the tapered bottom portion 34 and is symmetrically provided. Feeding port 36 and discharging port 37.
  • the frustum-shaped upper portion 32 is used for secondary steam concentration, and the cone-shaped bottom portion 34 is more conducive to the concentration of the crystal slurry formed by the crystal generated in the crystallizing portion 1 and is easy to lead out.
  • the outer deflector 4 includes opposite first and second ends 41 and 42.
  • the outer deflector 4 is located inside the crystallization section cylinder 3, and the first end 41 is fixedly connected to the straight middle portion 33 through a reducing diameter 43.
  • the intersection of the diameter 43 and the straight middle portion 33 is located above the clarified solution outlet 35, the second end 42 and the lower end 332 are on the same horizontal line, and the outer guide tube 4 is axisymmetric about the central axis 31.
  • the central baffle 5 includes a third end 51 and a fourth end 52 opposite to each other.
  • the central baffle 5 is located inside the outer baffle 4, and the horizontal level of the third end 51 is higher than the outer baffle 4 and the straight shape. Where the middle part 33 intersects, the liquid level at the upper part of the third end 51 is the evaporation interface 19, the height of the fourth end 52 in the horizontal plane is lower than the height of the second end 42 in the horizontal plane, and the central deflector 5 is axisymmetric about the central axis 31.
  • the bottom stirrer 6 is located inside the fourth end 52.
  • the secondary steam rising cylinder 7 has a cylindrical structure and is connected to the top end of the frustum-shaped upper portion 32 and is axisymmetric about the central axis 31.
  • the circulation pump 8 is located outside the cylinder body 3 of the crystallization section, and is connected to the inlet 36 and the clear solution inlet 35 through a pipe 9.
  • the inside of the center deflector 5 and the passage between the outer deflector 4 and the center deflector 5 form an inner circulation passage.
  • the internal circulation efficiency is high, which can maintain the density of the crystal slurry at the level of 30 to 40%, and can eliminate the high saturation area.
  • the saturation in each part of the crystallizer is relatively uniform and low, thereby enhancing the crystallizer production capacity.
  • the passage between the outer deflector 4 and the cylindrical middle portion 33 is a clarification zone 18, and the inner circulation passage, the clarification zone 18, the circulation pump 8 and the pipeline 9 form an outer circulation passage.
  • the outer circulation channel is used to eliminate excessive fine crystals and elutriation of product particle size, which can ensure the production of crystalline products with narrow particle size distribution, which can fully meet customer requirements for product particle size.
  • the condensing section 2 includes a condensing section cylinder 10 and an overflow weir 11, a first water blocking cap 12, a liquid folding ring 13 and a second water blocking cap 14 which are arranged in order from top to bottom inside the condensing section cylinder 10, and the condensing section cylinder
  • the body 10, the overflow weir 11, the first water-retaining cap 12, the liquid-retaining ring 13 and the second water-retaining cap 14 are all axially symmetrical about the central axis 31.
  • the condensation part 2 is located above the crystal part 1, and the condensation section cylinder 10
  • the bottom end covers the second steam rising cylinder 7 and is fixedly connected to the outer side of the frustum-shaped upper part 32.
  • the lower edge of the overflow weir 11 is sealedly connected to the condensing section cylinder 10, and the diameter of the upper edge of the overflow weir 11 is less than or equal to the first water retaining diameter.
  • the width of the baffle of the cap 12, the baffle ring 13 is located between the first baffle cap 12 and the second baffle cap 14, and the outer edge of the baffle ring 13 is fixed to the cylinder 10 of the condensation section.
  • the inner diameter is less than or equal to the width of the first water shield 12 and less than or equal to the width of the second water shield 14.
  • the condensing section cylinder 10 is provided with a cooling liquid injection port 101 at the overflow weir 11.
  • the bottom stirrer 6 is a push-type stirrer, which is used to push the mixed solution in the central draft tube 5 to the evaporation interface 19 on the upper part of the central draft tube 5 to improve the internal circulation efficiency in the internal circulation channel.
  • an upper part of the condensing section cylinder 10 is provided with a non-condensable gas outlet 102, which is located above the overflow weir 11 to discharge the non-condensable gas from the secondary steam out of the condensing section cylinder.
  • Body 10 is provided with a non-condensable gas outlet 102, which is located above the overflow weir 11 to discharge the non-condensable gas from the secondary steam out of the condensing section cylinder.
  • the pipeline outside the clarification solution introduction port 35 is connected to a fine crystal water pipe 351 for mixing the fine crystal water with the crystallization solution to eliminate fine crystals in the crystallization solution.
  • the lower part of the condensing section cylinder 10 is provided with a cooling and condensing mixed liquid outlet 103, and the height of the cooling and condensing mixed liquid outlet 103 from the ground is lower than the height of the secondary steam rising cylinder 7 from the ground.
  • the condensing section 2 further includes a liquid-sealing tank 15 and an atmospheric leg 16.
  • One end of the atmospheric leg 16 is connected to the cooling and condensing mixed liquid outlet 103, and the other end of the atmospheric leg 16 is connected to the liquid-sealing tank 15 for connecting the condensation section.
  • the cooling and condensing mixed liquid in the cylinder 10 is successfully drawn into the liquid-sealing tank 15, and the atmospheric leg 16 is filled with liquid and the height of the liquid column in the atmospheric leg 16 is between 10 and 20 meters. Relying on the gravity of the liquid column, the liquid seal tank 15 is automatically entered.
  • a cooling liquid deheating port 151 is provided at the bottom of the liquid sealing tank 15, and the cooling liquid deheating port 151 is connected to the cooling liquid injection port 101 through a circulation pipe.
  • the diameter of the outer guide tube 4 is twice the diameter of the central guide tube 5 to provide sufficient space for the outer circulation channel to eliminate excessive fine crystals and the granularity of the elutriation product.
  • the crystallizing section 1 further includes a product slurry pump 17, and the product slurry pump 17 is connected to the discharge port 37 through a pipe for drawing out the crystals generated by the crystallizing section 1.
  • the vertical vacuum crystallization device has a multi-stage series structure, and the outlet end of the circulation pump 8 of one of the two adjacent vertical vacuum crystallization devices is simultaneously with the other of the two adjacent vertical vacuum crystallization devices.
  • the inlet 36 is connected.
  • the invention is suitable for cooling crystals whose substance solubility changes greatly with temperature, such as the crystallization of solutions such as potassium chloride, ammonium sulfate, etc., and the solution that is preheated to a certain temperature in the previous stage (such as 90 ° C potassium chloride solution) and eliminates fine crystals.
  • the circulating liquid After the circulating liquid is mixed at the outlet of the circulating pump 8, it enters the central baffle 5 of the crystallizing part 1 and the suspension in the crystallizing part 1 is pushed together by a pusher to the evaporation interface 19 above the third end 51 of the central baffle 5 Under the action of vacuum, the solution (water) evaporates rapidly, absorbs the heat in the solution, reduces the temperature in the solution, makes the solution reach a certain saturation, the solute diffuses to the surface of the crystal, the crystal grows, and the large particle crystal flows along the center.
  • the cylinder 5 and the outer diversion cylinder 4 settle to the conical bottom 34 of the crystallizing section 1 and are sent to the next stage by the product slurry pump 17.
  • the small particles continue to circulate and grow in the internal circulation channel with the solution.
  • the solution in the clarification zone 18 of the external circulation overflows into the pipeline 9 of the external circulation channel.
  • the entrained fine crystals are dissolved in the pipeline 9 by the decrystallized water.
  • the solution is transported by the circulation pump 8 and most of it enters the crystallization section 1 to participate in the circulation. The rest The next section, to ensure the operation of the present level of the crystallizer.
  • the secondary steam generated by the evaporation interface 19 is separated into mist droplets during the ascent process. It passes through the secondary steam ascending cylinder 7 and enters the condensation part 2.
  • the cooling liquid overflowing from the overflow weir 11 passes through the first water cap 12
  • the baffle ring 13 and the second baffle cap 14 form three cooling liquid curtains (water curtains). After the secondary steam and the three condensation night curtains (water curtains) are fully condensed, the non-condensed non-condensable gas flows from the top.
  • the non-condensable gas outlet 102 is led out, and after the separated liquid droplets are separated, it enters a vacuum system and is discharged into the atmosphere.
  • the cooling liquid can be the low-temperature mother liquid after the slurry separation.
  • the multi-stage series crystallization final effect vertical vacuum crystallization device has low evaporation temperature and the secondary steam waste heat recovery value is not great. It is usually cooled by circulating water.
  • the mixed liquid condensed between the cooling liquid and the secondary steam overflows into the atmospheric leg 16 through the cooling and condensing mixed liquid inlet 103 and enters the liquid-sealing tank 15 and is sent through a circulation pipe as a cooling liquid or used for preparing a solution.
  • the invention uses vacuum to reduce the partial vapor pressure of the solution in the solution, so that the solution evaporates and takes away heat. It essentially relies on two effects of concentration and cooling to generate saturation, so that the solute crystals nucleate and grow.
  • the present invention combines the crystallization section 1 and the condensation section 2 into one device, which is different from other forms of the crystallization section 1 and the condensation section 2. Its main advantage is that it is not necessary to use pipes to introduce secondary steam from the crystallization section to the condensation section. Shorten the secondary steam flow path, eliminate the secondary steam overheating caused by pipeline resistance and increase the amount of coolant; eliminate the leakage of sealing points due to pipeline connection, and increase the pumping capacity of the vacuum system; at the same time, reduce the solution and The vacuum phase equilibrium evaporation temperature increases the evaporation of the solution and saves power consumption.
  • the equipment investment is saved, that is, the pipelines of the crystallizing section 1 and the condensing section 2 are saved; the supporting material of the condensing section 2 is saved; and the space for equipment installation is saved.
  • the crystallization part of the present invention is provided with a central baffle 5, a bottom agitator 6, and an outer baffle 4 to form an internal circulation channel.
  • the main advantages are: elimination of high saturation regions in the crystallization part 1, and The saturation is relatively uniform and low (undercooling can be controlled at ⁇ 1 ° C), which improves the evaporation intensity and strengthens the production capacity of the crystallizing unit 1.
  • the application of the propeller type agitator improves the internal circulation efficiency and reduces the crystal The probability of crushing and nucleation when colliding with the propeller agitator blade.
  • the propeller type agitator adopts variable frequency speed regulation, which is more helpful for adjusting the production load.
  • the advantages of the external circulation channel arrangement of the invention are: elimination of excessive fine crystals and elutriation of product particle size, ensuring the production of products with a very narrow particle size distribution, and the production of large particle size products with a particle size of 600 to 1200umr, which fully meets the needs of users. Requirements for different size distributions of product crystals.
  • the use of a large flow and low head axial flow pump as the circulation pump 8 effectively improves the external circulation volume, and is more helpful for the elutriation of the crystal size and the control of the crystal retention amount.
  • the effective volume of the crystallizing section 1 can be reduced by more than 30%, and the investment of equipment can be saved.
  • the invention has wide applicability, can be used for a variety of crystals such as adiabatic cooling method, evaporation method, direct contact method, and reaction method, and is more suitable for large-scale industrial crystal production.

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention provides a vertical vacuum crystallizing apparatus, comprising a crystallizing part and a condensing part. The crystallizing part is located below the condensing part. The crystallizing part comprises crystallizing section cylinder body, an outer flow guide cylinder, a central flow guide cylinder, a bottom stirrer, a secondary steam rising cylinder, a circulating pump, an inner circulating channel, and an outer circulating channel. The condensing part comprises a condensing section cylinder body as well as an overflow dam, a first water barrier cap, a liquid diverting ring, and a second water barrier cap which are disposed within the condensing section cylinder body in sequence from top to bottom. The advantages of the present invention are that: no heat exchanger is needed; the problems of serious scaling on an inner surface and scale cleaning do not exist; and because the vacuum operation pressure is close to the steam partial pressure of a solution, the operation is stable. The crystallizing part and the condensing part are combined to form one apparatus, such that a secondary steam flow path is shortened, and the seal point leakage caused by the increase of pipe connections are removed. The inner circulating channel removes a high saturation area in the crystallizing part, such that the saturations at different positions are even and low. The outer circulating channel removes excessive fine crystals and elutriates products with narrow particle size distribution.

Description

一种立式真空结晶装置Vertical vacuum crystallization device 技术领域Technical field
本发明涉及化工分离领域，具体涉及一种立式真空结晶装置。The invention relates to the field of chemical separation, in particular to a vertical vacuum crystallization device.
背景技术Background technique
结晶是指固体以晶体状态从气体、液体或熔融物中析出的过程，此过程是由热力学和动力学因素决定的，溶质要从溶液中析出，必须不断从外部获得能量，使溶液中溶液不断蒸发，使其达到饱和和过饱和，溶液未达到饱和时(处于稳定区)，溶质不会产生结晶，当溶液处于溶解度曲线和超溶解度曲线之间时(介稳区)，此时溶质结晶和溶解处于动态平衡，溶质不会自发成核析出，若有晶核进入就能长出晶体，此阶段极易受外界影响，即有无晶种、晶种大小、多少、有无搅拌、振动及杂质等因素，晶体的成长应控制在此区域内进行。溶液进入过饱和区(不稳定区)后，则会自发产生较多晶核。晶核的形成分为两类，无晶体存在的初级成核和有晶体存在的二次成核，在工业结晶过程中，通常控制二次成核,即流体的剪应力成核和接触成核,也就是选择合适的搅拌型式和转速。Crystallization refers to the process by which solids are precipitated from gases, liquids or melts in a crystalline state. This process is determined by thermodynamic and kinetic factors. To solute from a solution, energy must be continuously obtained from the outside to make the solution in the solution constantly Evaporate to make it saturated and supersaturated. When the solution is not saturated (in the stable region), the solute will not crystallize. When the solution is between the solubility curve and the supersolubility curve (metastatic region), the solute crystals and The dissolution is in a dynamic equilibrium, solutes will not spontaneously nucleate and precipitate. If crystal nuclei enter, crystals can grow out. This stage is extremely susceptible to external influences, such as the presence or absence of seeds, the size of seeds, the number of seeds, the presence of stirring, vibration and Factors such as impurities, crystal growth should be controlled within this region. After the solution enters the supersaturated region (unstable region), it will spontaneously generate more crystal nuclei. The formation of crystal nuclei can be divided into two types: primary nucleation without crystals and secondary nucleation with crystals. In industrial crystallization, secondary nucleation is usually controlled, that is, shear stress nucleation and contact nucleation of fluids. That is to choose the appropriate stirring type and speed.
根据化工单元操作普遍扩散理论分析，晶体的成长与以下因素有关：According to the general diffusion theory analysis of chemical unit operations, the growth of crystals is related to the following factors:
(1)晶体成长的推动力是溶液的过饱和浓度差和传递速度，过饱和溶液中的溶质扩散到晶核附近的相对静止液层，并穿过相对静止溶液层到达晶体表面嵌入晶面，使其晶体长大，并放出结晶热，热量再依靠扩散传递到溶液中。(1) The driving force for crystal growth is the supersaturation concentration difference and the transmission speed of the solution. The solute in the supersaturated solution diffuses into the relatively stationary liquid layer near the crystal nuclei, and passes through the relatively stationary solution layer to the crystal surface to embed the crystal plane. The crystal grows up and releases the heat of crystallization. The heat is then transferred to the solution by diffusion.
(2)溶液的温度，在相同的时间和相同的过饱和浓度差条件下，温度越高，溶液粘度越低，溶液的扩散速度越快，晶体的成长速度也快，越容易得到粒径 较大的晶体。(2) The temperature of the solution. At the same time and under the same supersaturation concentration difference, the higher the temperature, the lower the solution viscosity, the faster the solution's diffusion rate, and the faster the crystal growth rate. Big crystals.
(3)循环溶液流量，当蒸发量一定时同，循环溶液的流量和溶液的过饱和度成反比函数关系，而循环流量又确定了蒸发结晶器各部位的流速大小，流速大易引起晶体之间、晶体与器壁之间碰撞加剧，致使晶体破碎成二次晶核的可能性增大，对产品粒径影响也很大；流速小，不利于晶体的生长，因此要有适当的循环流量。(3) The circulating solution flow rate is the same when the evaporation amount is constant. The circulating solution flow rate and the solution's supersaturation are inversely proportional to each other, and the circulating flow rate determines the flow velocity of the various parts of the evaporation crystallizer. The collision between the crystal and the wall of the device is intensified, which increases the possibility of the crystal breaking into secondary crystal nuclei and has a great impact on the particle size of the product. The small flow rate is not conducive to the growth of the crystal, so an appropriate circulation flow rate is required. .
(4)晶浆浓度，在其它条件一定的前提下，晶浆浓度高则蒸发结晶器内晶体保有量多，晶体停留时间增长，有利于溶液过饱和度的消除和晶体成长，但晶浆浓度过高，晶体之间、晶体与器壁之间碰撞机率增多，晶体被破碎成二次晶核的机率也多，对晶体成长也不利，所以应当控制适当的晶体浓度，一般固液比控制在20％。(4) Crystal slurry concentration. Under other conditions, if the concentration of the crystal slurry is high, the crystal retention in the crystallizer will increase, and the crystal residence time will increase, which is beneficial to the elimination of solution supersaturation and crystal growth. If it is too high, the chance of collision between crystals, between the crystal and the wall will increase, and the probability of crystals being broken into secondary crystal nuclei will increase, which is also detrimental to crystal growth. Therefore, the appropriate crystal concentration should be controlled. Generally, the solid-liquid ratio is controlled at 20%.
(5)细晶消除，晶浆中细微结晶太多，过分消化了溶液过饱和度，影响其它晶体的生长，也不利于后续工序的分离，且商业用途太小，需要注入消晶水，溶解细微晶体，以控制粒数密度，产生较粗晶体产品。(5) Elimination of fine crystals, too many fine crystals in the crystal slurry, over-digestion of the solution's supersaturation, affecting the growth of other crystals, and not conducive to the separation of subsequent processes, and the commercial use is too small, it is necessary to inject crystal water Fine crystals to control grain density and produce coarser crystal products.
目前应用较多的结晶方法是采用强制外循环，料液自循环管下部加入，与离开结晶室底部的晶浆混合后，由泵送往加热室。晶浆在加热室内升温(通常为2～6℃)，但不发生蒸发。热晶浆进入结晶室后沸腾，使溶液达到过饱和状态，于是部分溶质沉积在悬浮晶粒表面上，使晶体长大。作为产品的晶浆从循环管上部排出。强制循环蒸发结晶器生产能力大，但由于该结晶器内部无搅拌装置，使得浆料的混合度变差，导致产品的粒度分布较宽；而且由于该设备中存在外循环冷却，所以其冷却管会比较容易结垢。At present, the most commonly used crystallization method is to use forced external circulation. The feed liquid is added from the lower part of the circulation tube, mixed with the crystal slurry leaving the bottom of the crystallization chamber, and then pumped to the heating chamber. The crystal slurry is heated in a heating chamber (usually 2 to 6 ° C), but evaporation does not occur. The hot crystal slurry boils after entering the crystallization chamber, so that the solution reaches a supersaturated state, so part of the solute is deposited on the surface of the suspended grains, and the crystal grows. The crystal slurry as a product is discharged from the upper part of the circulation pipe. The forced circulation evaporation crystallizer has a large production capacity, but because there is no stirring device in the crystallizer, the mixing degree of the slurry becomes poor, resulting in a wide particle size distribution of the product; and because of the external circulation cooling in the device, its cooling pipe Will be easier to scale.
发明内容Summary of the Invention
为解决上述问题，本发明提出了一种立式真空结晶装置。To solve the above problems, the present invention proposes a vertical vacuum crystallization device.
本发明的技术方案是：一种立式真空结晶装置，其特征在于包括:结晶部和冷凝部；The technical solution of the present invention is: a vertical vacuum crystallization device, which is characterized by comprising: a crystallization part and a condensation part;
所述结晶部包括结晶段筒体、外导流筒、中心导流筒、底搅拌器、二次蒸汽上升筒、循环泵、内循环通道和外循环通道；The crystallization part includes a crystallization section cylinder, an outer deflector, a central deflector, a bottom stirrer, a secondary steam rising cylinder, a circulation pump, an inner circulation channel and an outer circulation channel;
所述结晶段筒体是具有中心轴的轴对称结构，包括依次相连的锥台形上部、直筒形中部以及锥形底部，所述直筒形中部包括上端和下端，所述锥台形上部的大圆底面与所述上端相连，所述锥形底部的底面与所述下端相连，所述直筒形中部的中间位置开设有澄清溶液引出口，所述锥形底部上以所述中心轴为对称轴，对称地开设有入料口和出料口；The crystallization section cylinder is an axisymmetric structure with a central axis, and includes a frustum-shaped upper part, a straight middle part, and a tapered bottom connected in sequence. The straight middle part includes an upper end and a lower end, and a large round bottom surface of the frustum-shaped upper part and The upper end is connected, the bottom surface of the tapered bottom is connected to the lower end, a clear solution outlet is provided at the middle position of the straight cylindrical middle, and the central axis is a symmetrical axis on the tapered bottom, symmetrically There are inlet and outlet openings;
所述外导流筒包括相对的第一端和第二端，所述外导流筒位于所述结晶段筒体的内部，且所述第一端通过变径与所述直筒形中部固定连接，所述变径与所述直筒形中部交接处位于所述澄清溶液引出口的上方，所述第二端与所述直筒形中部的下端在同一水平线上，所述外导流筒以所述中心轴轴对称；The outer diversion cylinder includes first and second opposite ends, the outer diversion cylinder is located inside the crystallization section cylinder, and the first end is fixedly connected to the straight middle portion through a diameter reduction. The intersection of the reduced diameter and the straight middle portion is located above the outlet of the clear solution, the second end is on the same horizontal line as the lower end of the straight middle portion, and the outer diversion tube is based on the Central axis axisymmetric;
所述中心导流筒包括相对的第三端和第四端，所述中心导流筒位于所述外导流筒的内部，且所述第三端所在的水平面高于所述外导流筒与所述直筒形中部相交的位置，所述第三端上部的液面为蒸发界面，所述第四端在水平面的高度低于所述第二端在水平面的高度，所述中心导流筒以所述中心轴轴对称；The central baffle includes a third end and a fourth end opposite to each other. The central baffle is located inside the outer baffle, and a horizontal level at which the third end is located is higher than the outer baffle. At the position intersecting with the straight middle part, the liquid surface at the upper part of the third end is an evaporation interface, the height of the fourth end at the horizontal plane is lower than the height of the second end at the horizontal plane, and the central guide tube Axisymmetric about the central axis;
所述底搅拌器位于所述第四端的内部；The bottom stirrer is located inside the fourth end;
所述二次蒸汽上升筒为圆柱形结构且与所述锥台形上部的顶端相连且以所述中心轴轴对称；The secondary steam rising cylinder has a cylindrical structure and is connected to the top end of the frustum-shaped upper part and is axially symmetrical with the central axis;
所述循环泵位于所述结晶段筒体的外侧，且通过管道与所述入料口和所述澄清溶液引出口相连；The circulation pump is located outside the barrel of the crystallization section, and is connected to the feed inlet and the clear solution outlet through a pipeline;
所述中心导流筒的筒内、以及所述外导流筒与所述中心导流筒之间的通道形成所述内循环通道；The inner circulation channel of the central deflector and the channel between the outer deflector and the central deflector form the inner circulation channel;
所述外导流筒与所述圆柱形中部之间的通道为澄清区，所述内循环通道、所述澄清区、所述循环泵及所述管道形成所述外循环通道；A passage between the outer deflector and the cylindrical middle portion is a clarification zone, and the inner circulation passage, the clarification zone, the circulation pump, and the pipeline form the outer circulation passage;
所述冷凝部包括冷凝段筒体以及所述冷凝段筒体内部由上至下依次设置的溢流堰、第一挡水帽、折液环和第二挡水帽，所述冷凝段筒体、所述溢流堰、所述第一挡水帽、所述折液环以及所述第二挡水帽均以所述中心轴轴对称，所述冷凝部位于所述结晶部的上方，且所述冷凝段筒体底端罩住所述第二蒸汽上升筒固定连接于所述锥台形上部的外侧，所述溢流堰的下边沿与所述冷凝段筒体密封连接，所述溢流堰的上边沿直径小于等于所述第一挡水帽的挡水宽度，所述折液环位于所述第一挡水帽和所述第二挡水帽之间，且所述折液环的外边沿固定在所述冷凝段筒体上，所述折液环的内径小于等于所述第一挡水帽的挡水宽度，且小于等于所述第二挡水帽的挡水宽度，所述冷凝段筒体在所述溢流堰位置设有冷却液注入口。The condensing section includes a condensing section cylinder and an overflow weir, a first water-retaining cap, a liquid folding ring and a second water-retaining cap which are sequentially arranged from the top to the bottom of the condensing-section cylinder. , The overflow weir, the first water-retaining cap, the liquid-retaining ring, and the second water-retaining cap are all symmetrical about the central axis, and the condensation part is located above the crystal part, and The bottom end of the condensing section cylinder covers the second steam rising cylinder and is fixedly connected to the outer side of the frustum-shaped upper part. The lower edge of the overflow weir is sealedly connected to the condensing section cylinder. The overflow weir The diameter of the upper edge is less than or equal to the water-retaining width of the first water-retaining cap. The liquid-retaining ring is located between the first and second water-retaining caps. The edge is fixed on the cylinder of the condensation section, and the inner diameter of the liquid-retaining ring is less than or equal to the width of the first water retaining cap and less than or equal to the width of the second water retaining cap. The segment cylinder is provided with a cooling liquid injection port at the position of the overflow weir.
优选地，所述底搅拌器为推进式搅拌器，用以将所述中心导流筒内的混合溶液推进到所述中心导流筒上部的所述蒸发界面使内循环通道内的内循环效率提高。Preferably, the bottom stirrer is a push-type stirrer, which is used to push the mixed solution in the central draft tube to the evaporation interface on the upper part of the central draft tube to make the inner circulation efficiency in the inner circulation channel. improve.
优选地，所述冷凝段筒体的上部开设有不凝气体引出口，所述不凝气体引出口位于所述溢流堰的上方，用以将二次蒸汽中的不凝气排出所述冷凝段筒体。Preferably, an upper part of the condensing section cylinder is provided with a non-condensable gas outlet, and the non-condensable gas outlet is located above the overflow weir to discharge the non-condensable gas in the secondary steam from the condensation. Segment tube.
优选地，所述澄清溶液引出口外侧的管道上接有消细晶水管道，用以将消细晶水与结晶溶液混合，消除结晶溶液中的细晶。Preferably, the pipeline outside the outlet of the clarification solution is connected to a fine crystal water pipe, which is used to mix the fine crystal water with the crystallization solution to eliminate fine crystals in the crystallization solution.
优选地，所述冷凝段筒体下部开设有冷却冷凝混合液引出口，所述冷却冷 凝混合液引出口的距地高度小于所述二次蒸汽上升筒出汽端的距地高度。Preferably, a cooling condensate mixed liquid inlet is provided at the lower part of the barrel of the condensation section, and the height of the cooling condensate mixed liquid outlet from the ground is less than the height of the secondary steam rising tube from the ground.
优选地，所述冷凝部还包括液封槽和大气腿，所述大气腿的一端与所述冷却冷凝混合液引出口相连，所述大气腿的另一端接入所述液封槽，用以将所述冷凝段筒体内的冷却冷凝混合液成功引出至所述液封槽内，所述大气腿内充满液体且所述大气腿内液柱的距地高度在10～20米之间，用以使冷却冷凝混合液依靠液柱重力自动进入所述液封槽。Preferably, the condensing part further includes a liquid-sealing tank and an atmospheric leg, one end of the atmospheric leg is connected to the cooling and condensing mixed liquid outlet, and the other end of the atmospheric leg is connected to the liquid-sealing tank for The cooled and condensed mixed liquid in the condensing section cylinder was successfully drawn out into the liquid-sealed tank. The atmospheric leg was filled with liquid and the height of the liquid column in the atmospheric leg was between 10 and 20 meters. So that the cooling and condensing mixed liquid automatically enters the liquid-sealing tank by the gravity of the liquid column.
优选地，所述液封槽底部开设有冷却液去加热口，所述冷却液去加热口通过循环管道与所述冷却液注入口相连。Preferably, a cooling liquid de-heating port is provided at the bottom of the liquid sealing tank, and the cooling liquid de-heating port is connected to the cooling liquid injection port through a circulation pipe.
优选地，所述外导流筒的筒径是所述中心导流筒筒径的两倍，用以给所述外循环通道提供充足空间，以消除过量的细晶和淘洗产品的粒度。Preferably, the diameter of the outer diversion cylinder is twice the diameter of the central diversion cylinder to provide sufficient space for the outer circulation channel to eliminate excessive fine crystals and the granularity of the elutriation product.
优选地，所述结晶部还包括产品料浆泵，所述产品料浆泵通过管道与所述出料口相连，用以将所述结晶部产生的结晶引出。Preferably, the crystallizing section further includes a product slurry pump, and the product slurry pump is connected to the discharge port through a pipe, and is used for drawing out the crystals generated by the crystallizing section.
优选地，所述立式真空结晶装置为多级串联架构，相邻两个立式真空结晶装置的其中之一的循环泵的出口端同时与相邻两个立式真空结晶装置的其中之另一的入料口相连。Preferably, the vertical vacuum crystallization device is a multi-stage series structure, and the outlet end of the circulation pump of one of the two adjacent vertical vacuum crystallization devices is simultaneously with the other of the two adjacent vertical vacuum crystallization devices. The inlet of one is connected.
与现有技术相比，本发明的一种立式真空结晶装置主体设备简单，不需换热器，不存在内表面严重结垢，及结垢清理问题，从而影响生产能力；真空操作压力与溶液蒸汽分压相近，操作比较稳定。结晶部与冷凝部组合成一台设备，区别于其它形式的结晶蒸发器和冷凝器是分开的，其主要优点是：不需要用管道将二次蒸汽从结晶部引入冷凝部，缩短二次蒸汽流路，消除了因管道阻力导致二次蒸汽过热,而增加冷却液量；消除了因管道连接而增加的密封点泄漏，而增加真空***的抽气量；同时也降低了溶液与真空相平衡的蒸发温度,提高了溶 液的蒸发量，节约了动力能耗，同时节约了设备投资。本发明的内循环通道消除结晶器内高饱和度区域，结晶器内各处饱和度比较均匀，而且较低，提高了蒸发强度，强化了结晶器的生产能力，推进式搅拌器应用，提高了内循环效率，降低了晶体与桨叶碰撞破碎成核几率，搅拌器采用变频调速，更有助于调整生产负荷；外循环通道消除了过量的细晶，以及产品粒度的淘洗，保证能生产粒度分布很窄的产品。Compared with the prior art, the main equipment of a vertical vacuum crystallization device of the present invention is simple, does not require a heat exchanger, does not have serious scaling on the inner surface, and does not have scaling cleaning problems, thereby affecting production capacity; the vacuum operating pressure and The partial vapor pressure of the solution is similar, and the operation is relatively stable. The crystallization section and the condensation section are combined into one device, which is different from other forms of crystallization evaporator and condenser. Its main advantage is that it does not need to use pipes to introduce the secondary steam from the crystallization section to the condensation section, which shortens the secondary steam flow. Circuit, eliminating the secondary steam overheating caused by the resistance of the pipeline and increasing the amount of coolant; eliminating the leakage of the sealing point due to the connection of the pipeline, increasing the pumping capacity of the vacuum system; and reducing the equilibrium evaporation of the solution and the vacuum phase The temperature increases the evaporation of the solution, saves power consumption, and saves equipment investment. The internal circulation channel of the invention eliminates the high saturation area in the crystallizer, and the saturation in the crystallizer is relatively uniform and low, which improves the evaporation intensity, strengthens the production capacity of the crystallizer, and promotes the application of the agitator to improve Internal circulation efficiency reduces the chance of nucleation and fragmentation when crystals and blades collide. The mixer uses variable frequency speed regulation to help adjust the production load; the external circulation channel eliminates excessive fine crystals and the elutriation of product size to ensure Produces products with a narrow particle size distribution.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本发明的一种立式真空结晶装置的整体结构示意图。FIG. 1 is a schematic diagram of the overall structure of a vertical vacuum crystallization apparatus of the present invention.
具体实施方式detailed description
为使对本发明的目的、构造、特征、及其功能有进一步的了解，兹配合实施例详细说明如下。In order to further understand the purpose, structure, features, and functions of the present invention, the following detailed description is given in conjunction with the embodiments.
请参阅图1，图1为本发明的一种立式真空结晶装置整体结构示意图，如图1所示，本发明一实施例的立式真空结晶装置，包括结晶部1和冷凝部2。Please refer to FIG. 1. FIG. 1 is a schematic diagram of an overall structure of a vertical vacuum crystallization apparatus according to the present invention. As shown in FIG. 1, a vertical vacuum crystallization apparatus according to an embodiment of the present invention includes a crystallization section 1 and a condensation section 2.
结晶部1包括结晶段筒体3、外导流筒4、中心导流筒5、底搅拌器6、二次蒸汽上升筒7、循环泵8、内循环通道和外循环通道。The crystallization section 1 includes a crystallization section cylinder 3, an outer deflector 4, a center deflector 5, a bottom stirrer 6, a secondary steam riser 7, a circulation pump 8, an inner circulation channel, and an outer circulation channel.
结晶段筒体3是具有中心轴31的轴对称结构，包括依次相连的锥台形上部32、直筒形中部33以及锥形底部34，直筒形中部33包括上端331和下端332，锥台形上部32的大圆底面与上端331相连，锥形底部34的底面与下端332相连，直筒形中部33的中间位置开设有澄清溶液引出口35，锥形底部34上以中心轴31为对称轴，对称地开设有入料口36和出料口37。锥台形上部32用于二次蒸汽集中，锥形底部34更有利于结晶部1内产生的结晶形成的晶浆集中，便于引出。The crystalline section cylinder 3 is an axisymmetric structure with a central axis 31, and includes a frustum-shaped upper portion 32, a straight cylindrical middle portion 33, and a tapered bottom portion 34 connected in sequence. The straight cylindrical middle portion 33 includes an upper end 331 and a lower end 332, and the frustum-shaped upper portion 32 The large round bottom surface is connected to the upper end 331, the bottom surface of the tapered bottom portion 34 is connected to the lower end 332, a clear solution outlet 35 is provided in the middle of the straight cylindrical middle portion 33, and the central axis 31 is a symmetrical axis on the tapered bottom portion 34 and is symmetrically provided. Feeding port 36 and discharging port 37. The frustum-shaped upper portion 32 is used for secondary steam concentration, and the cone-shaped bottom portion 34 is more conducive to the concentration of the crystal slurry formed by the crystal generated in the crystallizing portion 1 and is easy to lead out.
外导流筒4包括相对的第一端41和第二端42，外导流筒4位于结晶段筒体 3的内部，且第一端41通过变径43与直筒形中部33固定连接，变径43与直筒形中部33交接处位于澄清溶液引出口35的上方，第二端42与下端332在同一水平线上，外导流筒4以中心轴31轴对称。The outer deflector 4 includes opposite first and second ends 41 and 42. The outer deflector 4 is located inside the crystallization section cylinder 3, and the first end 41 is fixedly connected to the straight middle portion 33 through a reducing diameter 43. The intersection of the diameter 43 and the straight middle portion 33 is located above the clarified solution outlet 35, the second end 42 and the lower end 332 are on the same horizontal line, and the outer guide tube 4 is axisymmetric about the central axis 31.
中心导流筒5包括相对的第三端51和第四端52，中心导流筒5位于外导流筒4的内部，且第三端51所在的水平面高于外导流筒4与直筒形中部33相交的位置，第三端51上部的液面为蒸发界面19，第四端52在水平面的高度低于第二端42在水平面的高度，中心导流筒5以中心轴31轴对称。底搅拌器6位于第四端52的内部。The central baffle 5 includes a third end 51 and a fourth end 52 opposite to each other. The central baffle 5 is located inside the outer baffle 4, and the horizontal level of the third end 51 is higher than the outer baffle 4 and the straight shape. Where the middle part 33 intersects, the liquid level at the upper part of the third end 51 is the evaporation interface 19, the height of the fourth end 52 in the horizontal plane is lower than the height of the second end 42 in the horizontal plane, and the central deflector 5 is axisymmetric about the central axis 31. The bottom stirrer 6 is located inside the fourth end 52.
二次蒸汽上升筒7为圆柱形结构且与锥台形上部32的顶端相连且以中心轴31轴对称。The secondary steam rising cylinder 7 has a cylindrical structure and is connected to the top end of the frustum-shaped upper portion 32 and is axisymmetric about the central axis 31.
循环泵8位于结晶段筒体3的外侧，且通过管道9与入料口36和澄清溶液引出口35相连。The circulation pump 8 is located outside the cylinder body 3 of the crystallization section, and is connected to the inlet 36 and the clear solution inlet 35 through a pipe 9.
中心导流筒5的筒内、以及外导流筒4与中心导流筒5之间的通道形成内循环通道。内循环效率高，可使晶浆密度保持在30～40％水平，并可以消除高饱和度区域，结晶器内各处饱和度比较均匀，而且较低，因而强化了结晶器的生产能力。The inside of the center deflector 5 and the passage between the outer deflector 4 and the center deflector 5 form an inner circulation passage. The internal circulation efficiency is high, which can maintain the density of the crystal slurry at the level of 30 to 40%, and can eliminate the high saturation area. The saturation in each part of the crystallizer is relatively uniform and low, thereby enhancing the crystallizer production capacity.
外导流筒4与圆柱形中部33之间的通道为澄清区18，内循环通道、澄清区18、循环泵8及管道9形成外循环通道。外循环通道用于消除过量的细晶，以及产品粒度的淘洗，保证了能生产粒度分布较窄的结晶产品，可充分满足客户对产品粒度的要求。The passage between the outer deflector 4 and the cylindrical middle portion 33 is a clarification zone 18, and the inner circulation passage, the clarification zone 18, the circulation pump 8 and the pipeline 9 form an outer circulation passage. The outer circulation channel is used to eliminate excessive fine crystals and elutriation of product particle size, which can ensure the production of crystalline products with narrow particle size distribution, which can fully meet customer requirements for product particle size.
冷凝部2包括冷凝段筒体10以及冷凝段筒体10内部由上至下依次设置的溢流堰11、第一挡水帽12、折液环13和第二挡水帽14，冷凝段筒体10、溢流 堰11、第一挡水帽12、折液环13以及第二挡水帽14均以中心轴31轴对称，冷凝部2位于结晶部1的上方，且冷凝段筒体10底端罩住第二蒸汽上升筒7固定连接于锥台形上部32的外侧，溢流堰11的下边沿与冷凝段筒体10密封连接，溢流堰11的上边沿直径小于等于第一挡水帽12的挡水宽度，折液环13位于第一挡水帽12和第二挡水帽14之间，且折液环13的外边沿固定在冷凝段筒体10上，折液环13的内径小于等于第一挡水帽12的挡水宽度，且小于等于第二挡水帽14的挡水宽度，冷凝段筒体10在溢流堰11位置设有冷却液注入口101。The condensing section 2 includes a condensing section cylinder 10 and an overflow weir 11, a first water blocking cap 12, a liquid folding ring 13 and a second water blocking cap 14 which are arranged in order from top to bottom inside the condensing section cylinder 10, and the condensing section cylinder The body 10, the overflow weir 11, the first water-retaining cap 12, the liquid-retaining ring 13 and the second water-retaining cap 14 are all axially symmetrical about the central axis 31. The condensation part 2 is located above the crystal part 1, and the condensation section cylinder 10 The bottom end covers the second steam rising cylinder 7 and is fixedly connected to the outer side of the frustum-shaped upper part 32. The lower edge of the overflow weir 11 is sealedly connected to the condensing section cylinder 10, and the diameter of the upper edge of the overflow weir 11 is less than or equal to the first water retaining diameter. The width of the baffle of the cap 12, the baffle ring 13 is located between the first baffle cap 12 and the second baffle cap 14, and the outer edge of the baffle ring 13 is fixed to the cylinder 10 of the condensation section. The inner diameter is less than or equal to the width of the first water shield 12 and less than or equal to the width of the second water shield 14. The condensing section cylinder 10 is provided with a cooling liquid injection port 101 at the overflow weir 11.
优选地，底搅拌器6为推进式搅拌器，用以将中心导流筒5内的混合溶液推进到中心导流筒5上部的蒸发界面19使内循环通道内的内循环效率提高。Preferably, the bottom stirrer 6 is a push-type stirrer, which is used to push the mixed solution in the central draft tube 5 to the evaporation interface 19 on the upper part of the central draft tube 5 to improve the internal circulation efficiency in the internal circulation channel.
优选地，冷凝段筒体10的上部开设有不凝气体引出口102，不凝气体引出口102位于溢流堰11的上方，用以将二次蒸汽中的不凝气排出所述冷凝段筒体10。Preferably, an upper part of the condensing section cylinder 10 is provided with a non-condensable gas outlet 102, which is located above the overflow weir 11 to discharge the non-condensable gas from the secondary steam out of the condensing section cylinder. Body 10.
优选地，澄清溶液引出口35外侧的管道上接有消细晶水管道351，用以将消细晶水与结晶溶液混合，消除结晶溶液中的细晶。Preferably, the pipeline outside the clarification solution introduction port 35 is connected to a fine crystal water pipe 351 for mixing the fine crystal water with the crystallization solution to eliminate fine crystals in the crystallization solution.
优选地，冷凝段筒体10下部开设有冷却冷凝混合液引出口103，冷却冷凝混合液引出口103的距地高度小于二次蒸汽上升筒7出汽端的距地高度。Preferably, the lower part of the condensing section cylinder 10 is provided with a cooling and condensing mixed liquid outlet 103, and the height of the cooling and condensing mixed liquid outlet 103 from the ground is lower than the height of the secondary steam rising cylinder 7 from the ground.
优选地，冷凝部2还包括液封槽15和大气腿16，大气腿16的一端与冷却冷凝混合液引出口103相连，大气腿16的另一端接入液封槽15，用以将冷凝段筒体10内的冷却冷凝混合液成功引出至液封槽15内，大气腿16内充满液体且大气腿16内液柱的距地高度在10～20米之间，用以使冷却冷凝混合液依靠液柱重力自动进入所述液封槽15。Preferably, the condensing section 2 further includes a liquid-sealing tank 15 and an atmospheric leg 16. One end of the atmospheric leg 16 is connected to the cooling and condensing mixed liquid outlet 103, and the other end of the atmospheric leg 16 is connected to the liquid-sealing tank 15 for connecting the condensation section. The cooling and condensing mixed liquid in the cylinder 10 is successfully drawn into the liquid-sealing tank 15, and the atmospheric leg 16 is filled with liquid and the height of the liquid column in the atmospheric leg 16 is between 10 and 20 meters. Relying on the gravity of the liquid column, the liquid seal tank 15 is automatically entered.
优选地，液封槽15底部开设有冷却液去加热口151，冷却液去加热口151 通过循环管道与冷却液注入口101相连。Preferably, a cooling liquid deheating port 151 is provided at the bottom of the liquid sealing tank 15, and the cooling liquid deheating port 151 is connected to the cooling liquid injection port 101 through a circulation pipe.
优选地，外导流筒4的筒径是中心导流筒5筒径的两倍，用以给外循环通道提供充足空间，以消除过量的细晶和淘洗产品的粒度。Preferably, the diameter of the outer guide tube 4 is twice the diameter of the central guide tube 5 to provide sufficient space for the outer circulation channel to eliminate excessive fine crystals and the granularity of the elutriation product.
优选地，结晶部1还包括产品料浆泵17，产品料浆泵17通过管道与出料口37相连，用以将结晶部1产生的结晶引出。Preferably, the crystallizing section 1 further includes a product slurry pump 17, and the product slurry pump 17 is connected to the discharge port 37 through a pipe for drawing out the crystals generated by the crystallizing section 1.
优选地，立式真空结晶装置为多级串联架构，相邻两个立式真空结晶装置的其中之一的循环泵8的出口端同时与相邻两个立式真空结晶装置的其中之另一的入料口36相连。Preferably, the vertical vacuum crystallization device has a multi-stage series structure, and the outlet end of the circulation pump 8 of one of the two adjacent vertical vacuum crystallization devices is simultaneously with the other of the two adjacent vertical vacuum crystallization devices. The inlet 36 is connected.
本发明适用于物质溶解度随温度变化较大的冷却结晶，如氯化钾、硫酸铵等溶液的结晶，前工段预热到一定温度的溶液(如90℃氯化钾溶液)与消除细晶外循环液在循环泵8出口混合后，进入结晶部1的中心导流筒5和结晶部1内悬浮液一起由推进式搅拌器推进到中心导流筒5的第三端51上部的蒸发界面19，在真空作用下,溶液(水)闪急蒸发，吸收溶液中热量，降低了溶液中温度，使溶液达到一定饱和度，溶质扩散到晶体表面，晶体长大，大颗粒晶体沿着中心导流筒5和外导流筒4沉降至结晶部1的锥形底部34晶浆区，通过产品料浆泵17采出送入下一段，小颗粒随溶液在内循环通道内继续循环长大，进入外循环的澄清区18的溶液，溢流入外循环通道的管道9，夹带的微细晶体在管道9中被消晶水溶解，溶液通过循环泵8的输送下，大部分进入结晶部1参加循环，其余部分进入下一段，以保证本结晶器的操作液位。The invention is suitable for cooling crystals whose substance solubility changes greatly with temperature, such as the crystallization of solutions such as potassium chloride, ammonium sulfate, etc., and the solution that is preheated to a certain temperature in the previous stage (such as 90 ° C potassium chloride solution) and eliminates fine crystals. After the circulating liquid is mixed at the outlet of the circulating pump 8, it enters the central baffle 5 of the crystallizing part 1 and the suspension in the crystallizing part 1 is pushed together by a pusher to the evaporation interface 19 above the third end 51 of the central baffle 5 Under the action of vacuum, the solution (water) evaporates rapidly, absorbs the heat in the solution, reduces the temperature in the solution, makes the solution reach a certain saturation, the solute diffuses to the surface of the crystal, the crystal grows, and the large particle crystal flows along the center. The cylinder 5 and the outer diversion cylinder 4 settle to the conical bottom 34 of the crystallizing section 1 and are sent to the next stage by the product slurry pump 17. The small particles continue to circulate and grow in the internal circulation channel with the solution. The solution in the clarification zone 18 of the external circulation overflows into the pipeline 9 of the external circulation channel. The entrained fine crystals are dissolved in the pipeline 9 by the decrystallized water. The solution is transported by the circulation pump 8 and most of it enters the crystallization section 1 to participate in the circulation. The rest The next section, to ensure the operation of the present level of the crystallizer.
蒸发界面19产生的二次蒸汽，在上升过程中分离出雾滴，通过二次蒸汽上升筒7，进入冷凝部2，溢流堰11上溢流而下的冷却液经过第一挡水帽12、折液环13、第二挡水帽14形成三道冷却液幕(水帘)，二次蒸汽与三道冷凝夜幕 (水帘)充分接触冷凝后，未被冷凝的不凝气，从顶部不凝气体引出口102引出，分离所携带的液滴后，进入真空***，排入大气。冷却液可以是料浆分离后的低温母液,多级串联结晶的末效立式真空结晶装置因蒸发温度较低，二次蒸汽余热回收价值不大，常用循环水冷却。冷却液与二次蒸汽冷凝后的混合液通过冷却冷凝混合液引出口103溢流入大气腿16，进入液封槽15，通过循环管道送上一段作冷却液，或用于配制溶液。The secondary steam generated by the evaporation interface 19 is separated into mist droplets during the ascent process. It passes through the secondary steam ascending cylinder 7 and enters the condensation part 2. The cooling liquid overflowing from the overflow weir 11 passes through the first water cap 12 The baffle ring 13 and the second baffle cap 14 form three cooling liquid curtains (water curtains). After the secondary steam and the three condensation night curtains (water curtains) are fully condensed, the non-condensed non-condensable gas flows from the top. The non-condensable gas outlet 102 is led out, and after the separated liquid droplets are separated, it enters a vacuum system and is discharged into the atmosphere. The cooling liquid can be the low-temperature mother liquid after the slurry separation. The multi-stage series crystallization final effect vertical vacuum crystallization device has low evaporation temperature and the secondary steam waste heat recovery value is not great. It is usually cooled by circulating water. The mixed liquid condensed between the cooling liquid and the secondary steam overflows into the atmospheric leg 16 through the cooling and condensing mixed liquid inlet 103 and enters the liquid-sealing tank 15 and is sent through a circulation pipe as a cooling liquid or used for preparing a solution.
本发明是利用真空降低溶液中溶液的蒸汽分压，使溶液蒸发并带走热量，实质上是同时依靠浓缩与冷却两种效应产生饱和度，使溶质晶体成核、生长。其相较于其它强迫外循环的结晶器(如FC、OLSO型结晶器)的优点为：主体设备简单，不需换热器，不存在内表面严重结垢，及结垢清理问题，从而影响生产能力；真空操作压力与溶液蒸汽分压相近，操作比较稳定。The invention uses vacuum to reduce the partial vapor pressure of the solution in the solution, so that the solution evaporates and takes away heat. It essentially relies on two effects of concentration and cooling to generate saturation, so that the solute crystals nucleate and grow. Compared with other crystallizers forced external circulation (such as FC, OLSO type crystallizers), its advantages are: the main equipment is simple, no heat exchanger is needed, there is no serious fouling on the inner surface, and the problem of fouling cleaning, which affects Production capacity; the vacuum operating pressure is similar to the partial pressure of the solution vapor, and the operation is relatively stable.
本发明将结晶部1与冷凝部2组合成一台设备，区别与其它形式的结晶部1与冷凝部2是分开的，其主要优点：不需要用管道将二次蒸汽从结晶部引入冷凝部，缩短二次蒸汽流路，消除了因管道阻力导致二次蒸汽过热,而增加冷却液量；消除了因管道连接而增加的密封点泄漏，而增加真空***的抽气量；同时也降低了溶液与真空相平衡的蒸发温度,提高了溶液的蒸发量，节约了动力能耗。节约了设备投资，即：节约了结晶部1与冷凝部2的管道；节约了冷凝部2安装支撑材料；节约设备安装的空间。The present invention combines the crystallization section 1 and the condensation section 2 into one device, which is different from other forms of the crystallization section 1 and the condensation section 2. Its main advantage is that it is not necessary to use pipes to introduce secondary steam from the crystallization section to the condensation section. Shorten the secondary steam flow path, eliminate the secondary steam overheating caused by pipeline resistance and increase the amount of coolant; eliminate the leakage of sealing points due to pipeline connection, and increase the pumping capacity of the vacuum system; at the same time, reduce the solution and The vacuum phase equilibrium evaporation temperature increases the evaporation of the solution and saves power consumption. The equipment investment is saved, that is, the pipelines of the crystallizing section 1 and the condensing section 2 are saved; the supporting material of the condensing section 2 is saved; and the space for equipment installation is saved.
本发明的结晶部内设中心导流筒5、底搅拌器6和外导流筒4，形成了内循环通道，其优点主要为：消除结晶部1内高饱和度区域，结晶部1内各处饱和度比较均匀，而且较低(过冷度能控制在<1℃)，提高了蒸发强度，强化了结晶部1的生产能力；推进式搅拌器应用，提高了内循环效率，降低了晶体与推进 式搅拌器桨叶碰撞破碎成核几率。推进式搅拌器采用变频调速，更有助于调整生产负荷。The crystallization part of the present invention is provided with a central baffle 5, a bottom agitator 6, and an outer baffle 4 to form an internal circulation channel. The main advantages are: elimination of high saturation regions in the crystallization part 1, and The saturation is relatively uniform and low (undercooling can be controlled at <1 ° C), which improves the evaporation intensity and strengthens the production capacity of the crystallizing unit 1. The application of the propeller type agitator improves the internal circulation efficiency and reduces the crystal The probability of crushing and nucleation when colliding with the propeller agitator blade. The propeller type agitator adopts variable frequency speed regulation, which is more helpful for adjusting the production load.
本发明的外循环通道的设置优点:消除了过量的细晶，以及产品粒度的淘洗，保证能生产粒度分布很窄的产品，能生产粒度达600～1200umr大粒径产品，充分满足用户对产品结晶不同粒度分布的要求。选用大流量低扬程的轴流泵作为循环泵8，有效提高了外循环量，更有助于晶体粒度的淘洗和晶体保有量的控制。相对于混合悬浮混合取出(MSMPR)结晶器，能使结晶部1的有效体积降低30％以上，节省设备的投资。The advantages of the external circulation channel arrangement of the invention are: elimination of excessive fine crystals and elutriation of product particle size, ensuring the production of products with a very narrow particle size distribution, and the production of large particle size products with a particle size of 600 to 1200umr, which fully meets the needs of users. Requirements for different size distributions of product crystals. The use of a large flow and low head axial flow pump as the circulation pump 8 effectively improves the external circulation volume, and is more helpful for the elutriation of the crystal size and the control of the crystal retention amount. Compared with the MSPPR crystallizer, the effective volume of the crystallizing section 1 can be reduced by more than 30%, and the investment of equipment can be saved.
本发明的适用性广，可用于绝热冷却法、蒸发法、直接接触法、及反应法等多种结晶，更适于大规模工业结晶生产。The invention has wide applicability, can be used for a variety of crystals such as adiabatic cooling method, evaporation method, direct contact method, and reaction method, and is more suitable for large-scale industrial crystal production.
本发明已由上述相关实施例加以描述，然而上述实施例仅为实施本发明的范例。必需指出的是，已揭露的实施例并未限制本发明的范围。相反地，在不脱离本发明的精神和范围内所作的更动与润饰，均属本发明的专利保护范围。The present invention has been described by the above related embodiments, but the above embodiments are merely examples for implementing the present invention. It must be noted that the disclosed embodiments do not limit the scope of the invention. On the contrary, changes and modifications made without departing from the spirit and scope of the present invention belong to the patent protection scope of the present invention.

Claims (10)

  1. 一种立式真空结晶装置，其特征在于包括:结晶部和冷凝部；A vertical vacuum crystallization device, comprising: a crystallization part and a condensation part;
    所述结晶部包括结晶段筒体、外导流筒、中心导流筒、底搅拌器、二次蒸汽上升筒、循环泵、内循环通道和外循环通道；The crystallization part includes a crystallization section cylinder, an outer deflector, a central deflector, a bottom stirrer, a secondary steam rising cylinder, a circulation pump, an inner circulation channel and an outer circulation channel;
    所述结晶段筒体是具有中心轴的轴对称结构，包括依次相连的锥台形上部、直筒形中部以及锥形底部，所述直筒形中部包括上端和下端，所述锥台形上部的大圆底面与所述上端相连，所述锥形底部的底面与所述下端相连，所述直筒形中部的中间位置开设有澄清溶液引出口，所述锥形底部上以所述中心轴为对称轴，对称地开设有入料口和出料口；The crystallization section cylinder is an axisymmetric structure with a central axis, and includes a frustum-shaped upper part, a straight middle part, and a tapered bottom connected in sequence. The straight middle part includes an upper end and a lower end, and a large round bottom surface of the frustum-shaped upper part and The upper end is connected, the bottom surface of the tapered bottom is connected to the lower end, a clear solution outlet is provided at the middle position of the straight cylindrical middle, and the central axis is a symmetrical axis on the tapered bottom, symmetrically There are inlet and outlet openings;
    所述外导流筒包括相对的第一端和第二端，所述外导流筒位于所述结晶段筒体的内部，且所述第一端通过变径与所述直筒形中部固定连接，所述变径与所述直筒形中部交接处位于所述澄清溶液引出口的上方，所述第二端与所述直筒形中部的下端在同一水平线上，所述外导流筒以所述中心轴轴对称；The outer diversion cylinder includes first and second opposite ends, the outer diversion cylinder is located inside the crystallization section cylinder, and the first end is fixedly connected to the straight middle portion through a diameter reduction. The intersection of the reduced diameter and the straight middle portion is located above the outlet of the clear solution, the second end is on the same horizontal line as the lower end of the straight middle portion, and the outer diversion tube is based on the Central axis axisymmetric;
    所述中心导流筒包括相对的第三端和第四端，所述中心导流筒位于所述外导流筒的内部，且所述第三端所在的水平面高于所述外导流筒与所述直筒形中部相交的位置，所述第三端上部的液面为蒸发界面，所述第四端在水平面的高度低于所述第二端在水平面的高度，所述中心导流筒以所述中心轴轴对称；The central baffle includes a third end and a fourth end opposite to each other. The central baffle is located inside the outer baffle, and a horizontal level at which the third end is located is higher than the outer baffle. At the position intersecting with the straight middle part, the liquid surface at the upper part of the third end is an evaporation interface, the height of the fourth end at the horizontal plane is lower than the height of the second end at the horizontal plane, and the central guide tube Axisymmetric about the central axis;
    所述底搅拌器位于所述第四端的内部；The bottom stirrer is located inside the fourth end;
    所述二次蒸汽上升筒为圆柱形结构且与所述锥台形上部的顶端相连且以所述中心轴轴对称；The secondary steam rising cylinder has a cylindrical structure and is connected to the top end of the frustum-shaped upper part and is axially symmetrical with the central axis;
    所述循环泵位于所述结晶段筒体的外侧，且通过管道与所述入料口和所述澄清溶液引出口相连；The circulation pump is located outside the barrel of the crystallization section, and is connected to the feed inlet and the clear solution outlet through a pipeline;
    所述中心导流筒的筒内、以及所述外导流筒与所述中心导流筒之间的通道形成所述内循环通道；The inner circulation channel of the central deflector and the channel between the outer deflector and the central deflector form the inner circulation channel;
    所述外导流筒与所述圆柱形中部之间的通道为澄清区，所述内循环通道、所述澄清区、所述循环泵及所述管道形成所述外循环通道；A passage between the outer deflector and the cylindrical middle portion is a clarification zone, and the inner circulation passage, the clarification zone, the circulation pump, and the pipeline form the outer circulation passage;
    所述冷凝部包括冷凝段筒体以及所述冷凝段筒体内部由上至下依次设置的溢流堰、第一挡水帽、折液环和第二挡水帽，所述冷凝段筒体、所述溢流堰、所述第一挡水帽、所述折液环以及所述第二挡水帽均以所述中心轴轴对称，所述冷凝部位于所述结晶部的上方，且所述冷凝段筒体底端罩住所述第二蒸汽上升筒固定连接于所述锥台形上部的外侧，所述溢流堰的下边沿与所述冷凝段筒体密封连接，所述溢流堰的上边沿直径小于等于所述第一挡水帽的挡水宽度，所述折液环位于所述第一挡水帽和所述第二挡水帽之间，且所述折液环的外边沿固定在所述冷凝段筒体上，所述折液环的内径小于等于所述第一挡水帽的挡水宽度，且小于等于所述第二挡水帽的挡水宽度，所述冷凝段筒体在所述溢流堰位置设有冷却液注入口。The condensing section includes a condensing section cylinder and an overflow weir, a first water-retaining cap, a liquid folding ring and a second water-retaining cap which are sequentially arranged from the top to the bottom of the condensing-section cylinder. , The overflow weir, the first water-retaining cap, the liquid-retaining ring, and the second water-retaining cap are all symmetrical about the central axis, and the condensation part is located above the crystal part, and The bottom end of the condensing section cylinder covers the second steam rising cylinder and is fixedly connected to the outer side of the frustum-shaped upper part. The lower edge of the overflow weir is sealedly connected to the condensing section cylinder. The overflow weir The diameter of the upper edge is less than or equal to the water-retaining width of the first water-retaining cap. The liquid-retaining ring is located between the first and second water-retaining caps. The edge is fixed on the cylinder of the condensation section, and the inner diameter of the liquid-retaining ring is less than or equal to the width of the first water retaining cap and less than or equal to the width of the second water retaining cap. The segment cylinder is provided with a cooling liquid injection port at the position of the overflow weir.
  2. 如权利要求1所述的立式真空结晶装置，其特征在于所述底搅拌器为推进式搅拌器，用以将所述中心导流筒内的混合溶液推进到所述中心导流筒上部的所述蒸发界面使内循环通道内的内循环效率提高。The vertical vacuum crystallization device according to claim 1, wherein the bottom stirrer is a push-type stirrer for advancing the mixed solution in the central draft tube to the upper part of the central draft tube. The evaporation interface improves the internal circulation efficiency in the internal circulation channel.
  3. 如权利要求1所述的立式真空结晶装置，其特征在于所述冷凝段筒体的上部开设有不凝气体引出口，所述不凝气体引出口位于所述溢流堰的上方，用以将二次蒸汽中的不凝气排出所述冷凝段筒体。The vertical vacuum crystallization device according to claim 1, characterized in that a non-condensable gas outlet is provided on the upper part of the cylinder of the condensation section, and the non-condensable gas outlet is located above the overflow weir for The non-condensable gas in the secondary steam is discharged from the cylinder of the condensation section.
  4. 如权利要求1所述的立式真空结晶装置，其特征在于所述澄清溶液引出口外侧的管道上接有消细晶水管道，用以将消细晶水与结晶溶液混合，消除结晶溶液中的细晶。The vertical vacuum crystallization device according to claim 1, characterized in that the pipeline outside the clarification solution outlet is connected with a fine crystal water pipe for mixing the fine crystal water and the crystallization solution to eliminate the crystallization solution. Fine crystals.
  5. 如权利要求1所述的立式真空结晶装置，其特征在于所述冷凝段筒体下部开设有冷却冷凝混合液引出口，所述冷却冷凝混合液引出口的距地高度小于所述二次蒸汽上升筒出汽端的距地高度。The vertical vacuum crystallization device according to claim 1, characterized in that a cooling condensate mixed liquid inlet is provided at the lower part of the barrel of the condensation section, and the height of the cooling condensate mixed liquid outlet from the ground is smaller than the secondary steam The height from the ground to the exit end of the rising cylinder.
  6. 如权利要求5所述的立式真空结晶装置，其特征在于所述冷凝部还包括液封槽和大气腿，所述大气腿的一端与所述冷却冷凝混合液引出口相连，所述大气腿的另一端接入所述液封槽，用以将所述冷凝段筒体内的冷却冷凝混合液成功引出至所述液封槽内，所述大气腿内充满液体且所述大气腿内液柱的距地高度在10～20米之间，用以使冷却冷凝混合液依靠液柱重力自动进入所述液封槽。The vertical vacuum crystallization device according to claim 5, characterized in that the condensing section further comprises a liquid-sealing tank and an atmospheric leg, and one end of the atmospheric leg is connected to the cooling and condensing mixed liquid outlet, and the atmospheric leg The other end is connected to the liquid-sealing tank, and is used to successfully draw the cooled and condensed mixed liquid in the condensing section cylinder into the liquid-sealing tank. The atmospheric leg is filled with liquid and the atmospheric leg liquid column. The height from the ground is between 10 and 20 meters, which is used to make the cooling and condensing mixed liquid automatically enter the liquid sealing tank by the gravity of the liquid column.
  7. 如权利要求6所述的立式真空结晶装置，其特征在于所述液封槽底部开设有冷却液去加热口，所述冷却液去加热口通过循环管道与所述冷却液注入口相连。The vertical vacuum crystallization device according to claim 6, characterized in that a cooling liquid deheating port is provided at the bottom of the liquid seal tank, and the cooling liquid deheating port is connected to the cooling liquid injection port through a circulation pipe.
  8. 如权利要求1所述的立式真空结晶装置，其特征在于所述外导流筒的筒径是所述中心导流筒筒径的两倍，用以给所述外循环通道提供充足空间，以消除过量的细晶和淘洗产品的粒度。The vertical vacuum crystallization device according to claim 1, characterized in that the diameter of the outer diversion cylinder is twice the diameter of the central diversion cylinder to provide sufficient space for the outer circulation channel, To eliminate excess fine grains and particle size of elutriation products.
  9. 如权利要求1所述的立式真空结晶装置，其特征在于所述结晶部还包括产品料浆泵，所述产品料浆泵通过管道与所述出料口相连，用以将所述结晶部产生的结晶引出。The vertical vacuum crystallizing device according to claim 1, wherein the crystallizing section further comprises a product slurry pump, and the product slurry pump is connected to the discharge port through a pipe for connecting the crystallizing section. The resulting crystals were extracted.
  10. 如权利要求1所述的立式真空结晶装置，其特征在于所述立式真空结晶装置为多级串联架构，相邻两个立式真空结晶装置的其中之一的循环泵的出口端同时与相邻两个立式真空结晶装置的其中之另一的入料口相连。The vertical vacuum crystallization device according to claim 1, characterized in that the vertical vacuum crystallization device has a multi-stage series structure, and an outlet end of a circulation pump of one of two adjacent vertical vacuum crystallization devices is simultaneously connected with The inlets of the other two vertical vacuum crystallizers are connected.
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