CN108905265A - Sodium vanadate Continuous Cooling Crystallization equipment and its production method - Google Patents

Sodium vanadate Continuous Cooling Crystallization equipment and its production method Download PDF

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Publication number
CN108905265A
CN108905265A CN201810830519.0A CN201810830519A CN108905265A CN 108905265 A CN108905265 A CN 108905265A CN 201810830519 A CN201810830519 A CN 201810830519A CN 108905265 A CN108905265 A CN 108905265A
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China
Prior art keywords
crystallizer
sodium vanadate
heat exchanger
pipeline
forecooler
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CN201810830519.0A
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Chinese (zh)
Inventor
张志�
郭坤
刘胜
曹芳利
房晓玲
上官菲菲
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Xian Aerospace Huawei Chemical and Biologic Engineering Co Ltd
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Xian Aerospace Huawei Chemical and Biologic Engineering Co Ltd
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Priority to CN201810830519.0A priority Critical patent/CN108905265A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0013Crystallisation cooling by heat exchange by indirect heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0059General arrangements of crystallisation plant, e.g. flow sheets
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D2009/0086Processes or apparatus therefor

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to sodium vanadate Continuous Cooling Crystallization equipment and its production method, equipment includes feed pump, forecooler, crystallizer, heat exchanger, thickener and centrifugal separating device;Crystallizer and heat exchanger pass through pipeline and circulating pump composition circulation, feed pump is set on the feed pipe before forecooler, and forecooler accesses the circulation by pipeline, which accesses thickener by pipeline from crystallizer, centrifugal separating device is accessed by pipeline again, accesses mother liquor tank finally by pipeline.The present invention uses Continuous Cooling Crystallization method, has stable input and output material and cooling process, and reduce cost of labor, can effectively improve production efficiency.

Description

Sodium vanadate Continuous Cooling Crystallization equipment and its production method
Technical field
The present invention relates to a kind of industrialized production sodium vanadate crystallization processes devices, and in particular to a kind of sodium vanadate continuous coo1ing Crystallizer and its production method.
Background technique
Vanadium is a kind of important strategy metal, has extensive purposes in steel, nonferrous metallurgy and chemical industry department.Generation at present In boundary there are about 90% vanadium be used for steel industry, remaining 10% be used for titanium alloy, vanadium cell, fine chemistry industry, catalyst, ceramics, light The production fields such as electricity.In steel industry, vanadium is mainly used as alloy addition to improve rigid intensity, toughness, ductility and heat-resisting The performances such as property.
Using the vanadium in sub-molten salt method high efficiency extraction vanadium slag mine, a conversion ratio of vanadium is made to reach 95% or more, but resulting Lye containing vanadium contains many substances, is one of the most effectual way for extracting vanadium in lye containing vanadium using crystallisation, and crystallized Journey condition is easily controllable, and crystallization temperature is low, and environmental pollution is small, and product purity height is, it can be achieved that continuous industrial production.Currently, Country facilities mostly use stirring pot type crystallizer, so that material is cooled down by outer jacketed and inner coil pipe, but the device has several masters Want defect:Separate unit treating capacity is small, and crystal size is uneven, and each batch poor product quality is anisotropic big;Crystallizer heat exchange is uneven, in device It exchanges heat on wall and coil pipe very fast, but is easy scale effect heat exchange rate on wall, coil pipe, heat-exchange time lengthens significantly;Stirring Pot type crystallizer belongs to periodic crystallisation device, and manual operation intensity is big etc..
Summary of the invention
The object of the present invention is to provide a kind of sodium vanadate Continuous Cooling Crystallization equipment and its production method, which can be real Continuous production is now industrialized, high degree of automation, occupied area is small, and cost of labor is low, obtained sodium vanadate crystal product granularity Uniformly, high-quality, yield is high.
The technical scheme adopted by the invention is as follows:
Sodium vanadate Continuous Cooling Crystallization equipment, it is characterised in that:
The equipment includes feed pump, forecooler, circulating pump, crystallizer, heat exchanger, thickener and centrifugal separating device;
Crystallizer and heat exchanger are recycled by pipeline and circulating pump composition, and feed pump is arranged on the feed pipe before forecooler, Forecooler accesses the circulation by pipeline, which accesses thickener by pipeline from crystallizer, then is accessed and be centrifuged by pipeline Separator accesses mother liquor tank finally by pipeline.
Heat exchanger is fixed tube-sheet exchanger, vertical placement, is arranged in parallel two groups, and a preparation and a use is respectively connected with circulation Pump;
Cooling water goes out from heat exchanger lower part into, top, and cooling water and material are at counterflow heat exchange.
It is provided with discharging pump on pipeline after crystallizer, thickener and mother liquor tank, respectively crystallizer discharging pump, thick Thick device discharging pump and mother liquor tank discharging pump.
Crystallizer pattern is Oslo type, which is cylindrical shape, and centre is coniform for what is shunk, and lowest part is Downspout is arranged in spherical shape, crystallizer inside.
Forecooler is spiral heat exchanger.
The production method of sodium vanadate Continuous Cooling Crystallization, it is characterised in that:
It is realized by following steps:
Material liquid first passes through forecooler pre-cooling by feed pump, subsequently into the circulating line between circulating pump and crystallizer, circulation Pump recycles material between crystallizer and heat exchanger, and heat exchanger keeps recycle stock temperature constant;
Crystallizer is cooling to obtain sodium vanadate magma, and magma is pumped into thickener and cached by crystallizer discharging pump, brilliant in thickener Slurries input centrifugal separating device carries out separation of solid and liquid operation.
Inlet amount is 20-30m3/ h, charging sodium vanadate mass concentration are 2%-5%, and temperature is 55-65 DEG C;
The mass ratio of internal circulating load and inlet amount is 50-200:1.
Load is identical as inlet amount, and crystallizer inside liquid level is kept to stablize, and drop temperature is 35-42 DEG C, and solid content is 3-15%, residence time 4-10h.
Cooling water and material carry out forced heat-exchanging in heat exchanger, and 25-35 DEG C of cold in-water temperature, temperature of charge 35-42 ℃。
70-80 DEG C of inlet temperature of forecooler thermal material.
The present invention has the following advantages that:
1, material liquid initially enters forecooler cooling, and the temperature difference of heat exchanger tube pass and shell side can be effectively reduced, prevent crystal quick-fried Hair nucleation blocking heat exchanger heat-exchanging tube.
2, heat exchanger uses vertical placement, a preparation and a use.Vertical heat exchanger can reduce crystal grain inside heat exchanger tube Residence time prevents plugging, and in the case where one, heat exchanger blocking, switching uses other one, guarantees production serialization.
3, circulating pump type is horizontal axial-flow pump, and the type impeller of pump acts on crystal grain breakage small, guarantee crystal Grain is complete, can obtain bulky grain crystal.Circulating pump makes solution forced circulation, also makes crystal particle diameter uniform.Circulating pump band frequency converter, Internal circulating load can be adjusted by way of adjusting the frequency of pump.
4, crystallizer uses Oslo pattern, and crystallizer is small to the destruction of crystal in this way without stirring, can guarantee that crystal is being tied Stabilization is grown up in brilliant device, guarantees biggish crystal grain.
5, crystallizer top direct tube section is equipped with overflow port, and overflow port is connect with mother liquor tank, keeps solid content in crystallizer low Supernatant overflow is gone out, and solid content in crystallizer is controlled.
Detailed description of the invention
Fig. 1 is sodium vanadate Continuous Cooling Crystallization complexes process flow chart;
Fig. 2 is forecooler scene photo;
Fig. 3 is sodium vanadate mold structure schematic diagram;
In figure, 1- feed pump;2- forecooler;3- circulating pump;4- crystallizer;5- heat exchanger;6- thickener;7- centrifuge separation dress It sets;8- mother liquor tank;9- crystallizer discharging pump;10- thickener discharging pump;11- mother liquor tank discharging pump.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
The present invention relates to sodium vanadate Continuous Cooling Crystallization equipment, for extracting vanadium from slag, belong to domestic initiation, it is described Equipment includes feed pump 1, forecooler 2, crystallizer 4, heat exchanger 5, thickener 6 and centrifugal separating device 7;Crystallizer 4 and heat exchange Device 5 is recycled by pipeline and the composition of circulating pump 3, and feed pump 1 is arranged on the feed pipe before forecooler 2, and forecooler 2 passes through pipe Road accesses the circulation, which accesses thickener 6 by pipeline from crystallizer 4, then accesses centrifugal separating device 7 by pipeline, Mother liquor tank 8 is accessed finally by pipeline.It is provided with discharging pump on pipeline after crystallizer 4, thickener 6 and mother liquor tank 8, point It Wei not crystallizer discharging pump 9, thickener discharging pump 10 and mother liquor tank discharging pump 12.
It is connected between crystallizer 4 and heat exchanger 5, heat exchanger 5 and circulating pump 3, circulating pump 3 and crystallizer 4 by pipeline, this A little connecting pipes are referred to as circulating line, and material liquid first passes through the pre-cooling of forecooler 2, then enters back into circulating line.Crystallizer 4 discharges Mouth and crystallizer discharging pump 8, crystallizer discharging pump 8 and thickener 6, thickener 6 and thickener discharging pump 9, thickener discharging pump 9 It is connect between centrifugal separation equipment 7 by pipeline, referred to as discharge pipe.
Heat exchanger 5 is fixed tube-sheet exchanger, and vertical placement is arranged in parallel two groups, and a preparation and a use is respectively connected with circulation Pump 3;Cooling water goes out from 5 lower part of heat exchanger into, top, and cooling water and material are at counterflow heat exchange.Fixed tube-sheet exchanger is one Kind is widely used in the common apparatus of the industries such as chemical industry, medicine, metallurgy, mainly has manufacture to be easy, production cost is low, cleaning side Just, adaptable, the advantages that treating capacity is big.
According to crystal property, it is Oslo type that the present invention, which chooses 4 pattern of crystallizer, which is cylindrical shape, in Between for shrink it is coniform, lowest part is spherical shape, and downspout is arranged inside crystallizer 4.The design can improve in crystallizer Flow of Goods and Materials state, is not easy to form dead zone;Appropriate to increase internal circulating load, crystal grain suspends in feed liquid, is in fluidization, can be with It avoids crystal adherent, guarantees that product granularity is uniform.
Forecooler 2 is spiral heat exchanger, is mainly pre-chilled to high-temperature feeding, prevents high-temperature feeding from leading to crystallizer 4 temperature unstabilitys;Spiral heat exchanger runner is generally cross-section rectangle, and flow dead zone, heat exchange is not present in fluid in channel Coefficient is big, and solid particle is not easy to plug runner, cooling water and thermal material counterflow heat exchange, good effect of heat exchange.
Based on above equipment, the production method of sodium vanadate Continuous Cooling Crystallization is realized by following steps:
Material liquid first passes through forecooler 2 by feed pump 1 and is pre-chilled, subsequently into the circulating line between circulating pump 3 and crystallizer 4, Circulating pump 3 recycles material between crystallizer 4 and heat exchanger 5, and heat exchanger 5 keeps recycle stock temperature constant;
The cooling of crystallizer 4 obtains sodium vanadate magma, and magma is pumped into thickener 6 and cached by crystallizer discharging pump 8, thickener 6 Interior magma input centrifugal separating device 7 carries out separation of solid and liquid operation.
Inlet amount is 20-30m3/ h, charging sodium vanadate mass concentration are 2%-5%, and temperature is 55-65 DEG C.Internal circulating load with into The mass ratio of doses should be depending on the difference of the crystal grain partial size of sodium vanadate in material, and ratio should be selected in 50-200: 1, target product granularity requirements are grown to guarantee crystalline particle.Load is identical as inlet amount, keeps 4 inside liquid of crystallizer Position is stablized, and drop temperature is 35-42 DEG C, solid content 3-15%, residence time 4-10h.
Cooling water and material carry out forced heat-exchanging in heat exchanger 5, and 25-35 DEG C of cold in-water temperature, temperature of charge 35-42 ℃.2 70-80 DEG C of thermal material inlet temperature of forecooler.
Forecooler 2 shown in Fig. 1 is spiral heat exchanger, cooling water and the thermal material counterflow heat exchange in heat exchanger.It is this kind of Type heat exchanger good heat-transfer, heat transfer efficiency is high, flow dead zone is not present in channel, equipment is strong from knot ability, and Non-fibrous is miscellaneous Object is difficult to retain, small accommodation area, it can accurately control material outlet temperature, prevents material that crystalline substance is precipitated in forecooler Body particle.Forecooler reduces the temperature of thermal material, can reduce the temperature difference of the cold and hot material of shell-and-tube heat exchanger, prevent temperature difference mistake Greatly, crystal outburst nucleation.
Crystallizer 4 of the present invention is Oslo pattern crystallizer, due to vanadic acid sodium crystal be it is needle-shaped, solution exists compared with large disturbances, Crystal grain is easily broken.If crystallizer uses the DTB pattern with agitating device, crystal fracture rate is big, crystal grain It is not easy to grow up.Oslo type crystallizer is stagewise crystallizer, and using circulating pump forced circulation, outer cooler is cooling, crystal grain Growth, the big product of available particle can be stablized in crystallizer.
Crystallizer top is cylindrical shape, and middle part is pyramidal structure, and lower part is hemispherical.Crystal grain be generally present under Portion, crystal size gradually becomes smaller from the bottom up, and discharge port is generally located on cone section, and three discharge ports are equidistantly arranged, discharge port There are certain angles to prevent discharging blockage with level.Since in vertical direction, crystal size is different, therefore open according to demand not Same discharge port obtains the crystal of variable grain size.
Embodiment 1:
This example demonstrates a kind of methods of Continuous Cooling Crystallization production vanadic acid sodium crystal.
75 DEG C of material temperature, sodium vanadate mass fraction 3.45%, alkali content 21.55g/L, raw material first pass through forecooler drop Temperature is cooled to 56 DEG C, subsequently into circulating line with heat exchanger, is cooled to 42 DEG C of maintenance temperature and is stablized.Forecooler, heat exchange Device is kept for 5-15 DEG C of temperature difference of heat exchanger, inlet amount 22m with 30 DEG C of cold in-water temperature3/ h, internal circulating load are 50 times of inlet amount, After cooling cycle 4-5h, solid content, the discharging when sodium vanadate mass fraction of solids reaches 3.25% is measured by sampling in sample tap.It keeps Continuous feeding and discharging maintains sodium vanadate crystallizer to pass in and out material balance.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.

Claims (10)

1. sodium vanadate Continuous Cooling Crystallization equipment, it is characterised in that:
The equipment includes feed pump(1), forecooler(2), circulating pump(3), crystallizer(4), heat exchanger(5), thickener(6)With Centrifugal separating device(7);
Crystallizer(4)And heat exchanger(5)Pass through pipeline and circulating pump(3)Composition circulation, forecooler(2)On feed pipe before Feed pump is set(1), forecooler(2)The circulation is accessed by pipeline, the circulation is from crystallizer(4)Thickener is accessed by pipeline (6), then centrifugal separating device accessed by pipeline(7), mother liquor tank is accessed finally by pipeline(8).
2. sodium vanadate Continuous Cooling Crystallization equipment according to claim 1, it is characterised in that:
Heat exchanger(5)For fixed tube-sheet exchanger, vertical placement is arranged in parallel two groups, and a preparation and a use is respectively connected with circulating pump (3);
Cooling water is from heat exchanger(5)Lower part goes out into, top, and cooling water and material are at counterflow heat exchange.
3. sodium vanadate Continuous Cooling Crystallization equipment according to claim 1, it is characterised in that:
Crystallizer(4), thickener(6)And mother liquor tank(8)Discharging pump is provided on pipeline later, respectively crystallizer discharges Pump(9), thickener discharging pump(10)With mother liquor tank discharging pump(12).
4. sodium vanadate Continuous Cooling Crystallization equipment according to claim 1, it is characterised in that:
Crystallizer(4)Pattern is Oslo type, which is cylindrical shape, and centre is coniform for what is shunk, and lowest part is Spherical shape, crystallizer(4)Inside setting downspout.
5. sodium vanadate Continuous Cooling Crystallization equipment according to claim 1, it is characterised in that:
Forecooler(2)For spiral heat exchanger.
6. the production method of sodium vanadate Continuous Cooling Crystallization, it is characterised in that:
It is realized by following steps:
Material liquid is by feed pump(1)First pass through forecooler(2)Pre-cooling, subsequently into circulating pump(3)With crystallizer(4)Between follow Endless tube road, circulating pump(3)Make material in crystallizer(4)With heat exchanger(5)Between recycle, heat exchanger(5)Keep recycle material temperature It spends constant;
Crystallizer(4)Cooling obtains sodium vanadate magma, crystallizer discharging pump(8)Magma is pumped into thickener(6)Caching is thick Thick device(6)Interior magma inputs centrifugal separating device(7)Carry out separation of solid and liquid operation.
7. the production method of sodium vanadate Continuous Cooling Crystallization according to claim 6, it is characterised in that:
Inlet amount is 20-30m3/ h, charging sodium vanadate mass concentration are 2%-5%, and temperature is 55-65 DEG C;
The mass ratio of internal circulating load and inlet amount is 50-200:1.
8. the production method of sodium vanadate Continuous Cooling Crystallization according to claim 7, it is characterised in that:
Load is identical as inlet amount, keeps crystallizer(4)Inside liquid level is stablized, and drop temperature is 35-42 DEG C, solid content 3- 15%, residence time 4-10h.
9. the production method of sodium vanadate Continuous Cooling Crystallization according to claim 6, it is characterised in that:
Cooling water and material are in heat exchanger(5)Progress forced heat-exchanging, 25-35 DEG C of cold in-water temperature, temperature of charge 35-42 ℃。
10. the production method of sodium vanadate Continuous Cooling Crystallization according to claim 6, it is characterised in that:
Forecooler(2)70-80 DEG C of thermal material inlet temperature.
CN201810830519.0A 2018-07-26 2018-07-26 Sodium vanadate Continuous Cooling Crystallization equipment and its production method Pending CN108905265A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114275813A (en) * 2021-12-30 2022-04-05 中国科学院过程工程研究所 Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system
CN114405049A (en) * 2021-12-09 2022-04-29 西安航天华威化工生物工程有限公司 System and method for crystallizing and purifying high-concentration lactic acid
CN114436779A (en) * 2020-10-30 2022-05-06 中国石油化工股份有限公司 Purification device of 1,4-cyclohexanedimethanol trans isomer and use method thereof

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CN107376399A (en) * 2017-08-17 2017-11-24 河钢股份有限公司承德分公司 A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate
CN209270883U (en) * 2018-07-26 2019-08-20 西安航天华威化工生物工程有限公司 A kind of sodium vanadate Continuous Cooling Crystallization equipment

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SU465209A1 (en) * 1973-09-10 1975-03-30 Предприятие П/Я В-2805 The method of crystallization solutions
CN202263415U (en) * 2011-09-17 2012-06-06 杭州天创环境科技股份有限公司 Freezing crystallization and tanner removing device for rich tanner saline water
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114436779A (en) * 2020-10-30 2022-05-06 中国石油化工股份有限公司 Purification device of 1,4-cyclohexanedimethanol trans isomer and use method thereof
CN114436779B (en) * 2020-10-30 2024-04-12 中国石油化工股份有限公司 Purification device for trans-isomer of 1,4-cyclohexanedimethanol and application method
CN114405049A (en) * 2021-12-09 2022-04-29 西安航天华威化工生物工程有限公司 System and method for crystallizing and purifying high-concentration lactic acid
CN114275813A (en) * 2021-12-30 2022-04-05 中国科学院过程工程研究所 Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system
CN114275813B (en) * 2021-12-30 2022-09-02 中国科学院过程工程研究所 Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system

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