CN205340185U - Continuous crystallization equipment of multistage high vacuum insulation flash distillation - Google Patents
Continuous crystallization equipment of multistage high vacuum insulation flash distillation Download PDFInfo
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- CN205340185U CN205340185U CN201520971491.4U CN201520971491U CN205340185U CN 205340185 U CN205340185 U CN 205340185U CN 201520971491 U CN201520971491 U CN 201520971491U CN 205340185 U CN205340185 U CN 205340185U
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Abstract
The utility model relates to a continuous crystallization equipment of multistage high vacuum insulation flash distillation. Establish ties by a plurality of crystallizers, its brilliant ware divide into straight section of thick bamboo section and down straight section of thick bamboo section, straight section of thick bamboo section diameter is little down, and it is big to go up straight section of thick bamboo section diameter, and two sections straight section of thick bamboos are connected by the reducing, it is short to go up straight section of thick bamboo section, down straight section of thick bamboo head, the crystallizer bottom is the W die bed, have the draft tube in the straight section of thick bamboo section in crystallizer lower part, the stirring of double -deck stirring rake is used in the top of crystallizer, stirring rake in stirring power consumption seat in the plane, and the diameter of stirring rake is less than the draft tube diameter, and the top layer stirring rake is higher than the draft tube, and the bottom layer stirring oar is located the draft tube lower part. The crystallizer top is connected with condenser and water ring vacuum pump, the turbidity appearance is equipped with to the crystallizer lower part. The matter entrance of crystallizers at different levels is located the draft tube bottom, is higher than lower floor's stirring rake, the discharge gate is located the crystallizer bottom, the discharging pipe of last one -level crystallizer is connected with centrifuge. Each crystallizer upper portion is provided with the shower. Production crystal particle diameter is even, and the outward appearance is better, and the crystal granularity is great and stable.
Description
Technical field
This utility model relates to a kind of continuous crystallisation device, is specially a kind of multi-stage vacuum adiabatic flash continuous crystallisation equipment；It is specifically related to a kind of multi-stage vacuum adiabatic flash continuous crystallisation equipment.
Background technology
In Chemical Manufacture, crystallization process is roughly divided into continuous crystallisation and two kinds of forms of periodic crystallisation.Batch crystallization process is disposable addition raw material, is then passed through different method for crystallising and obtains crystal, the crystallization process separated with mother solution by crystal for the last time.Periodic crystallisation due to the defect of its mode of operation, the problems such as the quality of product, highly dependent upon the experience of operator, so often leads to crystal thickness uneven, filtration difficulty.And owing to periodic crystallisation operation is discontinuous, its production efficiency is often not high enough, and occupation area of equipment is bigger.
Continuous crystallisation is then passed in crystallizer by lasting for material, and obtains the crystallization process of product continuously.For large-scale industrial crystallization process, the advantage of continuous crystallisation is in that, continuous crystallisation can pass through to control the operating condition of crystallizer not at the same level, can mother solution degree of supersaturation be controlled within Metastable zone, it is thus possible to effectively control nucleation, make the narrower particle size distribution of product, the quality of improving product.Due to continuous feed continuous discharge, greatly reduce the number of devices of crystallization process so that originally need the crystallization process of multiple periodic crystallisation device, as long as becoming a set of continuous crystallizing system.And due to continuous prodution, it is possible to reduce the manual operation impact on crystal, reduce the difference of different batches product, reach the purpose of stability contorting product quality.
Continuous crystallisation can be divided into the crystallization operations such as continuous coo1ing, continuous evaporation, adiabatic flash.For the continuous crystallisation of some system, owing to its mother liquid concentration is often higher, if adopting the mode of operation of Continuous Cooling Crystallization, knot wall problem often not easily solves.And due to continuous operation process, mother solution exists degree of supersaturation always, once produce knot wall, so knot wall will grow always, knot wall continues to grow up and can the stirring in crystallizer, heat transfer etc. be had a negative impact, and ultimately result in operation and can not run continuously, so how avoiding knot wall is the key issue of continuous crystallisation.Adiabatic flash is to take away mother solution heat by solvent vaporising under vacuum and make the process of mother solution crystallisation by cooling, its heat-transfer surface is at gas-liquid interface place, there is no the cooling surface of solid-liquid contact, and owing to the outer wall of crystallizer is enclosed with heat insulation layer, will not because of with environment heat exchange and cause wall place produce fouling, so knot wall problem can be avoided preferably, thus ensureing the continuous operation produced.
In Chinese patent CN200710130643.8 multifunctional multiple-effect automatic continuous evaporative crystallization technique and crystallizer, the technique describing a kind of continuous evaporation, the steam that it is characterized in that utilizing crystallizer to evaporate is as the Preheated steam of material liquid, thus reaching the purpose of energy efficient.But the magma outer circulation crystallizer that this patent uses needs additional steam heating evaporation, and this can make outer vaporizer easily tie wall, causes that continuous operation can not stable operation.
A kind of crystallizer for inorganic salt continuous crystallisation of Chinese patent CN203816265U inorganic salt continuous crystallisation device introduction, it is characterised in that employ outer circulation cooling and the apparatus-form of vacuum evaporation.But owing to there is outer circulation cooling in this equipment, so its cooling tube can be easier fouling, so that running continuously of device is affected.And due to the internal not stirring of this crystallizer, it is possible to the mixing situation of slurry can be made to be deteriorated, so that crystal size is deteriorated.
Summary of the invention
The purpose of this utility model is in that the defect for existing continuous crystallisation equipment, it is provided that one can promote crystalline product granularity and the multistage continuous vacuum adiabatic flash continuous crystallisation equipment of stability contorting crystal mass.
The technical scheme that this utility model provides is:
A kind of multi-stage vacuum adiabatic flash continuous device of the present utility model；Connected by multiple crystallizers；Its brilliant device is divided into direct tube section and lower direct tube section；Lower direct tube section diameter is little, and upper direct tube section diameter is big, and two sections of straight tubes are connected by reducing；Upper direct tube section is short, lower straight tube segment length；Crystalliser feet is at the bottom of W type；With guide shell in the direct tube section of crystallizer bottom；Stirring electricity consumption machine is positioned at the top of crystallizer, and stirring paddle uses Double-layer stirring paddle stirring, and the diameter of stirring paddle is less than draft tube diameter, and top layer stirring paddle is higher than guide shell, and bottom stirring paddle is positioned at guide shell bottom.
The diameter ratio of upper direct tube section and lower direct tube section is 1.2～2；The aspect ratio of upper direct tube section and lower direct tube section is 0.5～1；
The aspect ratio of guide shell height and lower direct tube section is 0.5～1, and draft tube diameter and lower direct tube section diameter ratio are 0.5～0.9；The ratio of diameter of stirring paddle and draft tube diameter is 0.6～0.95.
Crystallizer top is connected to condenser and water-ring vacuum pump；Crystallizer bottom is equipped with transmissometer.The material inlet of crystallizers at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle；Discharging opening is positioned at crystalliser feet；The discharge nozzle of afterbody crystallizer is connected with centrifuge.Each crystallizer top is provided with shower；The outer wall of crystallizer is enclosed with heat insulation layer.
Crystallizer of the present utility model, upper diameter is primarily to more greatly the fluctuation preventing vacuum, and owing to evaporating the liquid entrainment caused.Crystalliser feet is at the bottom of W type, and this is the design for reducing flow dead drawn through fluid Simulation.Stirring electricity consumption machine is positioned at the top of crystallizer, and stirring paddle uses Double-layer stirring paddle stirring, so can use relatively low speed of agitator and reach good mixed effect.Adopting top stirring is then to also there be reasonable mixed effect solid content is higher in mother solution.Crystallizer top is connected to condenser and water-ring vacuum pump for providing vacuum.Crystallizer bottom is equipped with transmissometer, and for measuring the slurry density within crystallizer, the operation for controlling crystallizer at different levels provides parameter.
The material inlet of crystallizers at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle.Discharging opening is positioned at crystalliser feet.The material liquid of first order crystallizer is injected by mother liquor tank.The discharging of upper level crystallizer is directly injected into next stage crystallizer by pump, by Flange joint between each pipeline.The discharge nozzle of afterbody crystallizer is connected with centrifuge, packaging warehouse-in after the centrifugal crystal drying obtained.If afterbody crystallizer needs Recycling Mother Solution, then the mother solution obtained after centrifugal is refilled in afterbody crystallizer by pump.
Each crystallizer top, all with shower, uses the water of evaporation in crystallizer to spray the knot wall at crystallizer inwall evaporating surface place, it is ensured that the operation of continuous operation.The outer wall of crystallizer is enclosed with heat insulation layer, for preventing due to low the caused crystallizer inwall knot wall of the temperature of environment.
Use this equipment to carry out continuous crystallisation and will have following beneficial effect:
1, the crystal particle diameter produced is uniform, and outward appearance is better, and crystal size is relatively big and granularity remains stable.
2, produce relatively Batch Process continuously and decrease the operating procedure of centre, reduce labor intensity, and can pass through to automatically control operation, reduce the product differences between batches owing to employee's operational issue causes.
3, promote crystallization process production efficiency, and greatly reduce number of devices.
4, method of the present utility model and equipment can also be generalized in the middle of the production of various inorganic salt and organic products.
Accompanying drawing explanation
Fig. 1 is a typical crystallizer of the present utility model；
Fig. 2 is two grades of continuous crystallization apparatus figure；
Fig. 3 is a level Four continuous crystallisation installation drawing；
Fig. 4 is three grades of continuous crystallization apparatus figure；
Fig. 5 is the product granularity that dibastic sodium phosphate uses that this technique continuous crystallisation obtains；
Fig. 6 is the dibastic sodium phosphate crystallogram using this technique to obtain；
1, spray header, 2, heat insulation layer, 3, charging aperture, 4, transmissometer, 5, motor, 6, guide shell, 7, stirring paddle, 8, discharging opening, 9, condenser, 10, raw material storage tank, 11, centrifugal pump, 12, crystallizer, 13, screw pump, 14, condensed water storage tank, 15, water-ring vacuum pump, 16, centrifuge.
Detailed description of the invention
Below in conjunction with drawings and Examples, detailed description of the invention of the present utility model is further described.Following example are only for clearly illustrating the technical solution of the utility model, and can not limit the protection domain of this patent with this.
Embodiment 1
As it is shown in figure 1, a kind of continuous vacuum adiabatic flash continuous crystalizer.Having heat insulation layer 2 outside crystallizer, the diameter of straight tube up and down of crystallizer is different, and the big lower diameter of upper diameter is little, and upper direct tube section diameter is 3.5 meters, and upper direct tube section height is 1.5 meters, and the diameter of lower direct tube section is 2.8 meters, and the height of lower direct tube section is 2 meters.The material of heat is entered the inside of guide shell 6 by charging aperture 3, and is stirred by double-deck major diameter stirring paddle 7, and the height of guide shell is 1.7 meters, and draft tube diameter is 1.83 meters, and the diameter of stirring paddle is 1.8 meters.Mix homogeneously in crystallizer, there is shower 1 on crystallizer top for spraying crystallizer inwall, to remove the knot wall at evaporating surface place.In crystallizer, the water of evaporation is condensed by condenser 9, and enters condensed water storage tank.Crystallizer bottom is provided with transmissometer 4, for monitoring the slurry density in crystallizer.
Embodiment 2
A kind of vacuum insulation flash distillation continuous crystallisation device, is connected by two crystallizers as shown in Figure 2.Crystallizer top is connected to condenser and water-ring vacuum pump；Crystallizer bottom is equipped with transmissometer.The material inlet of crystallizers at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle；Discharging opening is positioned at crystalliser feet；The discharge nozzle of afterbody crystallizer is connected with centrifuge.Each crystallizer top is provided with shower；The outer wall of crystallizer is enclosed with heat insulation layer.In storage tank 10, concentration is 17%, temperature is the dibastic sodium phosphate mother solution of 80 degree, entered in first order crystallizer 12 by centrifugal pump 11 according to the flow velocity of 7m3/h, the vacuum in first order crystallizer 12 is controlled so that in first order crystallizer 12, solid content is 6% by controlling the power of water-ring vacuum pump 15.And to control the mean residence time of slurry in first order crystallizer be 2h.The water flashed off in crystallizer is condensed by condenser 9, and is stored in condensed water storage tank 14, is squeezed in first order crystallizer by centrifugal pump 11 by the water in condensed water storage tank when evaporating surface place knot wall is more, washes away knot wall.Slurry in first order crystallizer is injected second level crystallizer 12 by pumping of screw pump 13, controls the vacuum in second level crystallizer 12 at 97kpa by controlling the power of water-ring vacuum pump 15, and the time of staying is 2h.The water flashed off in second level crystallizer 12 is condensed by condenser 9, and is stored in condensed water storage tank 14, is squeezed in the crystallizer of the second level by centrifugal pump 11 by the water in condensed water storage tank when evaporating surface place knot wall is more, washes away knot wall.Being injected in centrifuge by the slurry in the crystallizer of the second level by pump 13, the crystal after centrifugal is under room temperature after forced air drying, and packaging is put in storage.
Embodiment 3
A kind of vacuum insulation flash distillation continuous crystallisation device, is connected by four crystallizers as shown in Figure 3；Crystallizer top is connected to condenser and water-ring vacuum pump；Crystallizer bottom is equipped with transmissometer.The material inlet of crystallizers at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle；Discharging opening is positioned at crystalliser feet；The discharge nozzle of afterbody crystallizer is connected with centrifuge.Each crystallizer top is provided with shower；The outer wall of crystallizer is enclosed with heat insulation layer.Concentration in storage tank 10 is 23%, temperature is the dibastic sodium phosphate mother solution of 90 degree, entered in first order crystallizer 12 according to the flow velocity of 7m3/h by centrifugal pump 11, control the vacuum in first order crystallizer make in the first order crystallizer solid content 10% by controlling the power of water-ring vacuum pump 15.Controlling the mean residence time of slurry in first order crystallizer is 3h.Slurry in first order crystallizer 12 is injected second level crystallizer 12 by pumping of screw pump 13, controls the solid content in second level crystallizer 12 20% by controlling the power of water-ring vacuum pump 15.And to control the mean residence time of slurry in the crystallizer of the second level be 3h.Magma in second level crystallizer 12 is injected in third level crystallizer 12 by screw pump 13, controls the solid content of third level crystallizer 30% by controlling the power of water-ring vacuum pump 15.And to control the mean residence time of magma in third level crystallizer be 3h, the slurry of third level crystallizer 12 is injected fourth stage crystallizer by screw pump 13, the vacuum of fourth stage crystallizer is controlled at 97kpa by controlling the power of water-ring vacuum pump 15, in fourth stage crystallizer, the mean residence time of slurry is 3h, slurry in fourth stage crystallizer is injected in centrifuge 16 by screw pump 13, after the forced air drying under room temperature of the crystal after centrifugal, packaging warehouse-in.Mother liquor fraction after centrifugal is returned in fourth stage crystallizer by pump 11, it is ensured that the solid content in fourth stage crystallizer is lower than 50%.The product crystal particle size distribution obtained is shown in accompanying drawing 5, and the main granularity of crystal is 950 microns.Crystal outward appearance is shown in accompanying drawing 6.In the crystallizers at different levels of this technique, the operation of shower water is consistent with embodiment 2.
Embodiment 4
A kind of vacuum insulation flash distillation continuous crystallisation device, is connected by three crystallizers as shown in Figure 4；；Crystallizer top is connected to condenser and water-ring vacuum pump；Crystallizer bottom is equipped with transmissometer.The material inlet of crystallizers at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle；Discharging opening is positioned at crystalliser feet；The discharge nozzle of afterbody crystallizer is connected with centrifuge.Each crystallizer top is provided with shower；The outer wall of crystallizer is enclosed with heat insulation layer.In storage tank 10, concentration is 21.5%, and temperature is the dibastic sodium phosphate mother solution of 90 degree, centrifugal pump 11 enter in first order crystallizer 12 according to the flow velocity of 7m3/h, controls in first order crystallizer 12 solid content 8% by controlling the power of water-ring vacuum pump 15.And to control the mean residence time of slurry in first order crystallizer be 2.5h, first order crystallizer, slurry in first order crystallizer is injected second level crystallizer 12 by screw pump 13, controlling in the crystallizer of the second level that solid content is 20% by controlling the power of water-ring vacuum pump 15, in the crystallizer of the second level, the mean residence time of slurry is 2.5h.Slurry in the crystallizer of the second level is injected third level crystallizer 12 by screw pump 13, controls third level vacuum at 96kpa, time of staying 2.5h by controlling the power of water-ring vacuum pump 15.Slurry in the third level is injected in centrifuge 16 centrifugal, after the forced air drying under room temperature of the crystal after centrifugal, packaging warehouse-in.Mother liquor fraction after centrifugal is returned in third level crystallizer by centrifugal pump 11, it is ensured that the solid content in third level crystallizer is lower than 50%.In the crystallizers at different levels of this technique, the operation of shower water is consistent with embodiment 2.
Claims (6)
1. a multi-stage vacuum adiabatic flash continuous device；Connected by multiple crystallizers；It is characterized in that crystallizer is divided into direct tube section and lower direct tube section；Lower direct tube section diameter is little, and upper direct tube section diameter is big, and two sections of straight tubes are connected by reducing；Upper direct tube section is short, lower straight tube segment length；Crystalliser feet is at the bottom of W type；With guide shell in the direct tube section of crystallizer bottom；Stirring electricity consumption machine is positioned at the top of crystallizer, and stirring paddle uses Double-layer stirring paddle stirring, and the diameter of stirring paddle is less than draft tube diameter, and top layer stirring paddle is higher than guide shell, and bottom stirring paddle is positioned at guide shell bottom.
2. equipment as claimed in claim 1, is characterized in that the diameter ratio of upper direct tube section and lower direct tube section is 1.2～2；The aspect ratio of upper direct tube section and lower direct tube section is 0.5～1.
3. equipment as claimed in claim 1, is characterized in that the guide shell height aspect ratio with lower direct tube section is 0.5～1, and draft tube diameter and lower direct tube section diameter ratio are 0.5～0.9；The ratio of diameter of stirring paddle and draft tube diameter is 0.6～0.95.
4. equipment as claimed in claim 1, is characterized in that crystallizer top is connected to condenser and water-ring vacuum pump；Crystallizer bottom is equipped with transmissometer.
5. equipment as claimed in claim 1, is characterized in that the material inlet of crystallizer at different levels is positioned at bottom guide shell, higher than lower floor's stirring paddle；Discharging opening is positioned at crystalliser feet；The discharge nozzle of afterbody crystallizer is connected with centrifuge.
6. equipment as claimed in claim 1, is characterized in that each crystallizer top is provided with shower；The outer wall of crystallizer is enclosed with heat insulation layer.
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| CN201520971491.4U CN205340185U (en) | 2015-11-27 | 2015-11-27 | Continuous crystallization equipment of multistage high vacuum insulation flash distillation |
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| CN201520971491.4U CN205340185U (en) | 2015-11-27 | 2015-11-27 | Continuous crystallization equipment of multistage high vacuum insulation flash distillation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105435482A (en) * | 2015-11-27 | 2016-03-30 | 天津大学 | Multi-stage vacuum adiabatic flash continuous crystallization method and equipment |
| CN112678779A (en) * | 2021-02-02 | 2021-04-20 | 天津大学 | Preparation method of ammonium persulfate crystal |
| CN116492700A (en) * | 2023-06-30 | 2023-07-28 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
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2015
- 2015-11-27 CN CN201520971491.4U patent/CN205340185U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105435482A (en) * | 2015-11-27 | 2016-03-30 | 天津大学 | Multi-stage vacuum adiabatic flash continuous crystallization method and equipment |
| CN112678779A (en) * | 2021-02-02 | 2021-04-20 | 天津大学 | Preparation method of ammonium persulfate crystal |
| CN112678779B (en) * | 2021-02-02 | 2023-03-14 | 天津大学 | Preparation method of ammonium persulfate crystal |
| CN116492700A (en) * | 2023-06-30 | 2023-07-28 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
| CN116492700B (en) * | 2023-06-30 | 2023-09-12 | 上海中腾环保科技有限公司 | Graded flash evaporation equipment and process |
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