CN101658735B - Continuous vacuum crystallization device and application thereof - Google Patents

Continuous vacuum crystallization device and application thereof Download PDF

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Publication number
CN101658735B
CN101658735B CN2009103070607A CN200910307060A CN101658735B CN 101658735 B CN101658735 B CN 101658735B CN 2009103070607 A CN2009103070607 A CN 2009103070607A CN 200910307060 A CN200910307060 A CN 200910307060A CN 101658735 B CN101658735 B CN 101658735B
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China
Prior art keywords
crystallization
pump
crystallization kettle
vacuum
flow
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Expired - Fee Related
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CN2009103070607A
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Chinese (zh)
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CN101658735A (en
Inventor
赖成文
许章道
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Chengdu Hanneng Chemical Machinery Co Ltd
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Chengdu Hanneng Chemical Machinery Co Ltd
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Abstract

The invention discloses a continuous vacuum crystallization device and an application in the production of barium chloride, and the device comprises a crystallization pot, a raw material pump, a vacuum condensing recovery device, an electric heating temperature controlling device, a shaft flow pump and a bottom valve, wherein the bottom of the crystallization pot is in a conical shape, and the electric heating temperature controlling device is arranged at a place positioned above half height of the crystallization pot; the shaft flow pump is vertically arranged at the middle of the crystallization pot, the distance between the propeller of the pump and the top end of a conical body at the bottom of the crystallization pot is 1/3 time larger than the inner height of the crystallization pot, the propeller of the pump drives fluid raw materials upwards, and a liquid lifting pipe is arranged around the pump shaft of the shaft flow pump and the propeller of the pump; and the bottom of the crystallization pot can be also provided with a flow assisting device. The whole device is produced in enclosed environment, the process of crystallization is completed at one time, the device has continuous production process, high heating efficiency, stable fluid flow, stable and continuous crystallization, easy discharge for products and energy saving, and the device is not only suitable for large-scale industrial production, but also reduces environmental pollution and energy waste.

Description

A kind of continuous vacuum crystallization device and application thereof
Technical field
The present invention relates to a kind of chemical industry equipment, relate in particular to a kind of vacuum crystallization device and the application in Production of Barium Chloride thereof.
Background technology
Vacuum concentrating apparatus has concentration tank, vacuum condensation recover, liquid material pumps into concentration tank by feedstock pump, in concentration tank, heat, under the suction of vacuum condensation recover intermediate pump, concentrate, it need be finished crystallization one after another and concentrate, can not carry out continuously, particularly there is following shortcoming in it in Production of Barium Chloride:
1, can not produce continuously, the incompatibility large-scale industrial needs.
2, power consumption is high.Because the Production of Barium Chloride process is to need crystallization more than 4 times, its 4 crystallization cooling procedures are carried out under nature, cause energy loss.
Summary of the invention
The purpose of this invention is to provide a kind of continuous vacuum crystallization device, it has overcome above-mentioned shortcoming, and solves the discharge problem of product in the continuous flow procedure, and steam is recycled problem.Especially be applied in the Production of Barium Chloride process.The present invention realizes by following method:
The present invention is by crystallization kettle, the feedstock pump that is connected with crystallization kettle by pipeline, the vacuum condensation recover that is connected with crystallization kettle by pipeline, the electrical heating temperature regulating device, axial-flow pump, formations such as bottom valve, described crystallization kettle bottom is the centrum shape, and the centrum top connects the crystallization kettle bottom valve; The electrical heating temperature regulating device is installed in the crystallization kettle inner height and locates more than 1/2nd, axial-flow pump is vertically mounted on the middle part of crystallization kettle, impeller of pump should be greater than high by 1/3rd in the whole crystallization kettle apart from centrum top, crystallization kettle bottom, and the active force that impeller of pump drives material liquid upwards.
Pump shaft and impeller of pump at axial-flow pump are installed stalk on every side, the stalk upper and lower opening, stalk is fixed on the crystallization kettle top cover, impeller of pump is in the stalk under shed, stalk upwards flows material liquid from stalk under the effect of impeller of pump, arriving crystallization kettle top flows downward along the crystallization kettle wall from the outside of stalk again, raw material liq separately flows up and down and makes the interior liquid flow of crystallization kettle stable, the efficiency of heating surface improves, crystallization-stable, because impeller of pump has certain distance apart from the crystallization kettle bottom, the crystalline particle that grows up to is no longer stirred by impeller of pump because of gravity sinks to greatly in the crystallization kettle centrum, and nucleus and mother liquor drive by axial-flow pump and continue circulation.
Be provided with bottom crystallization kettle flow-aiding device can also be installed, flow-aiding device comprises that a fluid pump and an end are connected the pipeline of other end outlet over against the crystallization kettle bottom valve with the fluid pump, and the distance of pipe outlet and crystallization kettle bottom valve is 100~500mm.The fluid pump can be an air compressor, blows out product by compressed air; Also can be the liquid charging stock pump, discharge by the supersaturated solution boosting product that pumps corresponding crystallization.
The electrical heating temperature regulating device is installed in the crystallization kettle inner height and locates more than 1/2nd, be looped around the crystallization kettle periphery of inner wall, the electrical heating temperature regulating device makes crystallization kettle upper and lower temperature difference and helps evaporation and crystallization, and electrical heating is common quartz heater, temperature regulating device ordinary procedure temperature regulating device.
The vacuum condensation recover comprises condenser, vavuum pump, compositions such as preferred water odd test jet vacuum pump, water odd test jet vacuum pump is simple in structure, utilize jet vacuum pump current suction evaporation steam, water jets and evaporation recycle-water are merged to be used, reduce evaporation recycle-water gathering-device, make the anhydrous waste of production process.
When material liquid enters crystallization kettle, the heating temperature control, continue vacuum filtration, along with water evaporates, concentration of raw material progressively increases, its time-continuing process solute is by nucleus one brilliant clock (adding crystal seed for the first time brings out) thermal crystalline, when concentration is thickened to that saturated solution is critical spends, crystal in the supersaturated solution because of gravitational settling in crystallization kettle bottom, continue initiate material liquid under axial-flow pump drives and in the crystallization kettle solution mix to be incorporated in and form the still center in the crystallization kettle and upwards flow, arrive the still top again along downward the circulating of still wall, crystalline hydrate is opened flow-aiding device and is helped row along with the generation of crystallization continues to discharge through the crystallization kettle bottom valve when discharge is smooth.
All commercially available chemical industry equipments such as above-mentioned raw materials pump, crystallization kettle, pipeline, electrical heating temperature regulating device, condenser, vavuum pump, water odd test jet vacuum pump, axial-flow pump, bottom valve, air compressor, fluid pump.
The present invention especially produces in the barium chloride crystalline product at the barium chloride material liquid and uses, and the heating temperature control preferred 103 ℃, continued vacuum 10~30Kpa suction filtration at 100 ℃~113 ℃ during it was produced.
Compared with prior art, the beneficial effect that the present invention has is: device can be produced in enclosed environment, accessory substance obtains recycling, crystallization process is once finished, reduce evaporation concentration equipment quantity, production process is continuous, electrical heating temperature regulating device and axial-flow pump make crystallization kettle efficiency of heating surface height, liquid flow is stable, crystallization-stable is continuous, the product of producing is easily discharged, and the product impurity content is low, apparatus of the present invention energy savings, adapt to the large-scale industrial production needs, reduced the waste of pollution and resource to greatest extent.
Description of drawings
Fig. 1 is the crystallization kettle structural representation;
Fig. 2 is the crystallization kettle structural representation that flow-aiding device is installed.
The specific embodiment
Embodiment 1: in conjunction with Fig. 1, continuous vacuum crystallization device comprises crystallization kettle 21, by pipeline and crystallization kettle inlet 17 feedstock pumps that are connected 5, by pipeline and the crystallization kettle steam outlet 18 vacuum condensation recovers 10 that are connected, electrical heating temperature regulating device 13, axial-flow pump 6,7,8, bottom valve 14 formations such as grade, described crystallization kettle bottom 22 is the centrum shape, and the centrum top connects crystallization kettle bottom valve 14; Electrical heating temperature regulating device 13 is installed in the crystallization kettle inner height and locates more than 1/2nd, axial-flow pump 6,7,8 is vertically mounted on the middle part of crystallization kettle, impeller of pump 6 should be greater than high by 1/3rd in the whole crystallization kettle apart from centrum top, crystallization kettle bottom, and the active force that impeller of pump 6 drives material liquids upwards.
Material liquid enters crystallization kettle 21 by feedstock pump 5 by crystallization kettle inlet 17, the heating temperature control, continuing vacuum filtration and axial flow drives, steam is extracted out and the condensation reuse through vacuum condensation recover 10 by outlet 18, along with water evaporates, concentration of raw material progressively increases, its time-continuing process solute is by nucleus one brilliant clock (can add crystal seed for the first time brings out) thermal crystalline, when concentration is thickened to that saturated solution is critical spends, crystal in the supersaturated solution because of gravitational settling in crystallization kettle centrum bottom 22, continue initiate material liquid at axial-flow pump 6,7, under 8 drivings and the mixed crystallization kettle 21 interior formation still centers that are incorporated in of the interior solution of crystallization kettle make progress mobile, arrive the still top again along downward the circulating of still wall, the adding speed of control material liquid makes crystallization reach balance, and crystalline hydrate is along with the generation of crystallization continues to discharge through crystallization kettle bottom valve 14.
Above-mentioned crystallization kettle centrum bottom 22 helps gravitational settling, collection, the discharge of crystal; Electrical heating temperature regulating device 13 is installed in the crystallization kettle inner height and locates more than 1/2nd, is looped around the crystallization kettle periphery of inner wall, and the interior solution of material liquid that new benefit is gone into and crystallization kettle mixes and obtains heating, and the mixed solution of heating flows downward and helps the sedimentation of separating out of crystal; Axial-flow pump 6,7,8 makes the mixed interior still center that forms of crystallization kettle that is incorporated in of the interior solution of crystallization kettle make progress mobile in the middle part of being vertically mounted on crystallization kettle, arrive the still top again along downward the circulating of still wall, it makes, and solution has afterflow moving in the crystallization kettle, adds thermal balance, and crystal is separated out the sedimentation continous-stable; Extract steam out in conjunction with vacuum condensation recover 10, whole process realizes once heating up, continuous evaporation, concentrated, and continuous crystallisation goes out product.
In crystallization kettle 21, around axial-flow pump pump shaft 8 and the impeller of pump 6 stalk 7 is installed, stalk 7 upper and lower openings 9,11, stalk 7 is fixed on crystallization kettle 21 top covers, impeller of pump 6 is in stalk 7 under sheds 11, stalk 7 upwards flows material liquid from stalk 7 under the effect of impeller of pump 6, arrive crystallization kettle 21 tops and flow downward along crystallization kettle 21 walls from the outside of stalk 7 again, raw material liq separately flows up and down and makes the efficiency of heating surface improve crystallization-stable.
The vacuum condensation recover comprises condenser, vavuum pump, compositions such as preferred water odd test jet vacuum pump, water odd test jet vacuum pump is simple in structure, utilizes jet vacuum pump current suction evaporation steam, jet and evaporation recycle-water are merged use, reduce evaporation recycle-water gathering-device.
Embodiment 2: in conjunction with Fig. 2, repeat embodiment 1 by described same steps as, but the crystallization kettle bottom is provided with flow- aiding device 19,20 is installed also, flow-aiding device comprises that a fluid pump 20 and an end are connected other end outlet 19 pipelines over against crystallization kettle bottom valve 14 with fluid pump 20, and pipe outlet 19 is 100~500mm with the distance of crystallization kettle bottom valve.Fluid pump 20 is raw material liq pumps, discharges by the supersaturated solution boosting product that pumps corresponding crystallization.Crystal in the production process in the supersaturated solution because of gravitational settling in crystallization kettle centrum bottom 22, open flow- aiding device 19,20 rows of helping when smooth when discharging.
Embodiment 3: preparation barium chloride material liquid, to remove the hydration barium chloride material liquid of impurity and filtration through feedstock pump 5 input crystallization kettles 21 through oxidation, electrical heating temperature regulating device 13 heating temperature controls make crystallization kettle 21 interior temperature remain on 100 ℃~113 ℃, preferred 103 ℃, vacuum condensation recover 10 pump up water steam and condensation reuse, vacuum keeps 10 ~ 30Kpa, material liquid is at axial-flow pump 6,7,8 drivings form the still center down and upwards flow in crystallization kettle 21, arrive the still top again along downward the circulating of still wall, concentration of raw material progressively increases, its time-continuing process solute is by nucleus one brilliant clock (adding crystal seed for the first time brings out) thermal crystalline, when concentration is thickened to that 32 Baumes are critical spends, barium chloride crystal in the supersaturated solution because of gravitational settling in crystallization kettle bottom 22, crystallization kettle bottom 22 is the centrum shape, the centrum top connects crystallization kettle bottom valve 14, the barium chloride crystalline hydrate is along with the generation of crystallization continues to discharge through crystallization kettle bottom valve 14, material liquid continues to mend goes into to make production to carry out continuously, the adding speed of control material liquid makes crystallization reach balance, saturated barium chloride crystalline hydrate filters, its a small amount of filtrate is returned evaporative crystallization, the white crystal solid content is barium chloride, and further the processing dehydration can be produced a water barium chloride, anhydrous barium chloride and other barium products.
To produce 1.5 ten thousand tons of barium chlorides per year is example: 1.4~1.8 meters of crystallization kettle diameters, preferred 1.4 meters; High 5~6 meters, preferred 5 meters; The centrum height is 1/2nd of a crystallization kettle diameter; In the normal productive process, the material liquid input speed is per hour 11 cubic metres, 600~700 kilowatts of electrical heating powers, 500-550 rev/min of control axial flow revolution speed, then can reach in 0.5 ℃ of heating part, crystallization kettle top and the bottom subsidence part temperature difference, this helps crystal grain grows up and sedimentation, and is no longer stirred by the axial-flow pump impeller of pump, the continuation circulation of nucleus and mother liquor; This moment, 8 cubic metres/hour of the water yields were reclaimed in the whole process of production evaporation, discharged 3 cubic metres/hour in mother liquor, and barium chloride 2000kg/ hour, realization flush distillation crystallization was produced continuously.

Claims (8)

1. a continuous vacuum crystallization device mainly comprises crystallization kettle, and the feedstock pump that is connected with crystallization kettle by pipeline is by the vacuum condensation recover that pipeline is connected with crystallization kettle, electrical heating temperature regulating device, axial-flow pump, bottom valve; It is characterized in that: described crystallization kettle bottom is the centrum shape, and the centrum top connects the crystallization kettle bottom valve; The electrical heating temperature regulating device is installed in the crystallization kettle inner height and locates more than 1/2nd; Axial-flow pump is vertically mounted on the middle part of crystallization kettle, and impeller of pump should be greater than high by 1/3rd in the whole crystallization kettle apart from centrum top, crystallization kettle bottom, and the active force that impeller of pump drives material liquid upwards.
2. continuous vacuum crystallization device according to claim 1 is characterized in that: axial-flow pump comprises pump shaft, impeller of pump and stalk, and the stalk upper and lower opening is fixed on the crystallization kettle top cover, and impeller of pump is in the stalk under shed.
3. continuous vacuum crystallization device according to claim 1 is characterized in that: the vavuum pump of vacuum condensation recover is a water odd test jet vacuum pump.
4. according to claim 1,2 or 3 each described continuous vacuum crystallization devices, it is characterized in that: in the crystallization kettle bottom flow-aiding device is set, flow-aiding device comprises that a fluid pump and an end are connected the pipeline of other end outlet over against the crystallization kettle bottom valve with the fluid pump.
5. continuous vacuum crystallization device according to claim 4 is characterized in that: the distance of flow-aiding device pipe outlet and crystallization kettle bottom valve is 100~500mm.
6. continuous vacuum crystallization device according to claim 4 is characterized in that: the temperature of described continuous vacuum crystallization device when heating in vacuum concentrates is 100 ℃~113 ℃.
7. continuous vacuum crystallization device according to claim 4 is characterized in that: the vacuum of described continuous vacuum crystallization device when heating in vacuum concentrates is 10~30Kpa.
8. the application of continuous vacuum crystallization device in producing barium chloride, comprise the preparation of barium chloride material liquid, Concentrated and crystallized in vacuum and centrifugal finished product step is characterized in that: the Concentrated and crystallized in vacuum of barium chloride material liquid is carried out in the described continuous vacuum crystallization device of above-mentioned arbitrary claim continuously.
CN2009103070607A 2009-09-15 2009-09-15 Continuous vacuum crystallization device and application thereof Expired - Fee Related CN101658735B (en)

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Application Number Priority Date Filing Date Title
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CN101658735B true CN101658735B (en) 2011-11-09

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Publication number Priority date Publication date Assignee Title
CN102641607A (en) * 2012-03-11 2012-08-22 甘肃蓝科石化高新装备股份有限公司 Vaporization crystallizer device with mechanical vapor compressor
CN105879424B (en) * 2014-09-30 2017-11-07 海洲环保集团有限公司 Vacuum shwoot cooling continuous crystallisation device
CN107837557B (en) * 2017-12-13 2019-11-19 清远佳致新材料研究院有限公司 The continuous crystallizing system and its technique of a kind of coarse granule, low water-insoluble cobaltous sulfate

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