CN104192917B - Nickel-cobalt sulfate continuous-crystallizing process - Google Patents
Nickel-cobalt sulfate continuous-crystallizing process Download PDFInfo
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Abstract
The invention discloses a nickel sulfate hexahydrate crystal and cobalt sulfate heptahydrate crystal continuous-crystallizing process which comprises the following steps: firstly carrying out MVR evaporation concentration on a high-purity solution produced through an extraction procedure to 30%-39%, and secondly continuously cooling and crystallizing through an improved cooling type internal-circulating continuous crystallizer; continuously discharging crystal slurry from the bottom of the crystallizer for centrifugal solid-liquid separation; and continuously drying a crystal product at low temperature to produce product crystals with large granularity and uniform size distribution, and recovering a mother solution to an evaporation process. Compared with the traditional periodic crystallization process, the nickel sulfate hexahydrate crystal and cobalt sulfate heptahydrate crystal continuous-crystallizing process disclosed by the invention has the advantages of low evaporation energy consumption, fewer crystallization control process parameters, stability in operation, high automation degree, high production efficiency and the like and is easy to control, and operators are reduced.
Description
Technical field
The invention belongs to sulfate industrial production technology field, particularly to a kind of sulfate continuous crystallisation technique.
Background technology
Industrial production nickel cobalt sulfate is usually that weak solution is concentrated into saturation through single-action, two effects and triple effect evaporation technique
Afterwards, then carry out one-pot intermittent cooling crystallization produce obtain.This technique has the disadvantage in that 1, evaporation technology energy consumption is big；2nd, crystallize
Process control parameters are many, automaticity is low, low production efficiency, the difficulty that controls are big, personnel qualifications are high.
Content of the invention
It is an object of the invention to overcoming defect present in prior art, provide a kind of six hydration nickel sulfate and seven hydrations
Cobaltous sulfate continuous crystallisation technique.Mainly comprise the steps:
(1) evaporation and concentration: according to the solubility curve of nickel sulfate or cobalt sulfate solution, will be extracted using mvr evaporation technology
Take the high-purity weak solution evaporation and concentration of 15%～25% (wt%) of operation output to 28%～39%, drop temperature is 80～90
DEG C, 50～60% standard matchmaker for traditional triple effect evaporation, can be saved using mvr evaporation technology, energy-saving effect shows
Write；
(2) Continuous Cooling Crystallization: using external water cooling type interior circulation continuous crystalizer, the 80 of output in rate-determining steps 1
～90 DEG C of concentrated solutions are with 1～10m3The flow of/h enters external cooler, and external cooler is connected with crystallizer circulation line, leads to
Cross feed liquid circulating load 900～1500m that circulating pump controls cooler3/ h, by the speed of agitator of VFC crystallizer 85
～108r/min, makes crystallizer interior circulation amount in 1000～2000m3In/h range of flow, in crystallizer, crystal is in suspension
State, this is conducive to the growth of crystal.Magma temperature in crystallizer is 32～45 DEG C, and the temperature of charge of cooler is higher than crystallizer
1～5 DEG C of magma temperature, the continuous six hydration nickel sulfate magma discharged of crystalliser feet discharging opening or Cobalt monosulfate heptahydrate magma are extremely
Next procedure.For controlling crystal size, crystallizer is provided with fine crystal elimination device, for by the supernatant containing a large amount of fine crystals
Liquid returns evaporization process dissolving, thus ensureing growing up of crystal in crystallizer, it is 0～3m that supernatant returns liquid measure3/h.
(3) filtration drying: by the magma of above-mentioned steps 2 output with, after centrifuge filtration separation, crystal uses vibratory liquefaction again
Bed continuous low temperature Wind Volume is dried to obtain that granularity is big, pack after the crystal product of even particle size distribution, and baking temperature is 50～
60 DEG C, mother solution returns evaporization process.
For controlling cooler in above-mentioned steps 2 to crystallize and scab due to nickel sulfate or cobaltous sulfate, affect heat transfer effect, increase
The technique of cooler recirculated cooling water inner loop and equipment, control the temperature stabilization of cooler heat exchange wall as far as possible, reduced
The fluctuation of saturation, thus controlling crystal amount of precipitation and the speed of separating out on cooler heat exchange wall, recirculated cooling water self-loopa amount
For 200～300m3/ h, recirculated cooling water gives back to coolant-temperature gage and is respectively 32 DEG C and 38 DEG C.
For controlling vibrated fluidized bed continuous low temperature drying effect in above-mentioned steps 3, it is to avoid uneven drying, crystal is reunited etc.
Problem, the present invention increased vibrating material-distributing device before exsiccator entrance, on the one hand wet crystal uniformly can scatter again
Enter exsiccator；On the other hand adopt vibrating material-distributing device, the broken of crystal can also be prevented effectively from.
Further, the mass percent of the high-purity sulphuric acid nickel described in step 1 or cobaltous sulfate concentrated solution is respectively preferably
30～39%.
Further, in step 2, crystallizer magma and cooler material temperature difference are preferably 1～3 DEG C.
The present invention, for traditional triple effect evaporation, can save 50～60% standard matchmaker using mvr evaporation technology,
Energy-saving effect is notable, and achieves the continuous prodution of technique, simple to operation.
Brief description
Fig. 1: continuous crystallisation process chart
Wherein: 1- crystallizer；2- cooler；3a- coolant circulation pump；3b- recirculated water self-circulating pump；4- circulates water storage tank；
5- valve；6- valve；7- valve；8- valve；9- valve.
Specific embodiment
Embodiment 1:
Control valve 7 aperture, Solute mass is than 80～90 DEG C of nickel sulfate concentrated solutions for 37%～39% with 1～4m3/h
Flow enter cooling circulation line.Control coolant circulation pump p01 variable-frequency governor, adjustment pump flow be 900～
1100m3/h.Control valve 6 aperture, circulating cooling water flow is 40～85m3/ h, makes cooler drop temperature be 33～38 DEG C.
Control crystallization agitator jb01 variable-frequency governor, adjustment stirring lifting rate is 1000～1200m3/ h, makes crystal be in suspension
State, this is conducive to the classification of crystal to grow up, and in crystallizer, magma temperature is 32～35 DEG C.Valve 9 is closed.Control valve 5 aperture,
Crystallizer magma discharging is 1～4m3/ h, and after centrifugation and drying 75～80% crystal particle diameter 1～2mm six hydrations
Nickel sulfate hexahydrate crystal product.
Embodiment 2:
Control valve 7 aperture, Solute mass is than 80～90 DEG C of cobaltous sulfate concentrated solutions for 30%～33% with 4～8m3/h
Flow enter cooling circulation line.Control coolant circulation pump p01 variable-frequency governor, adjustment pump flow be 1100～
1250m3/h.Control valve 6 aperture, circulating cooling water flow is 80～97m3/ h, makes cooler drop temperature be 35～40 DEG C.
Control crystallization agitator jb01 variable-frequency governor, adjustment stirring lifting rate is 1200～1500m3/ h, makes crystal be in suspension
State, this is conducive to the classification of crystal to grow up, and in crystallizer, magma temperature is 32～38 DEG C.Control valve 9 aperture, fine crystal elimination liquid
Back amount is 1～2m3/h.Control valve 5 aperture, crystallizer magma discharging is 4～8m3/ h, and after centrifugation and drying 80～
85% crystal particle diameter is in the Cobalt monosulfate heptahydrate crystal product of 1～2mm.
Embodiment 3:
Control valve 7 aperture, Solute mass is than 80～90 DEG C of nickel sulfate concentrated solutions for 38%～39% with 8～10m3/h
Flow enter cooling circulation line.Control coolant circulation pump p01 variable-frequency governor, adjustment pump flow be 1250～
1500m3/h.Control valve 6 aperture, circulating cooling water flow is 85～106m3/ h, makes cooler drop temperature be 39～45 DEG C.
Control crystallization agitator jb01 variable-frequency governor, adjustment stirring lifting rate is 1500～1800m3/ h, makes crystal be in suspension
State, in crystallizer, magma temperature is 35～43 DEG C.Control valve 9 aperture, fine crystal elimination liquid back amount is 2～3m3/h.Control valve
Door 5 apertures, crystallizer magma discharging is 8～10m3/ h, and after centrifugation and drying 85～90% crystal particle diameter 1～
The six hydration nickel sulfate product of 2mm.
In above-described embodiment, the self-loopa flow 200～300m of recirculated cooling water3/ h, cooler is scabbed due to heat exchange wall
And the cycle of cleaning during shutdown is more than 3 months.
The foregoing is only presently preferred embodiments of the present invention, not the present invention is made with any pro forma restriction, appoint
What makes any simple modification, equivalent variations and modification according to the technical spirit of the present invention to above example, belongs to this
In the range of bright technical scheme.
Claims (6)
1. a kind of nickel cobalt sulfate continuous crystallisation technique it is characterised in that:
(1) will be dense to nickel sulfate or cobaltous sulfate with mvr technique evaporation and concentration to 15～25% high-purity sulphuric acid nickel or cobalt sulfate solution
Degree enters circulation line close to the solution of saturation, enters external cooler cooling with circulation fluid, close to full after described concentration
The solution temperature of sum is 80～90 DEG C, and mass percent is 30～39%；
(2) solution after circulation fluid and evaporation and concentration enters back into crystallizer after external cooler cools down, and cooler material goes out
Material temperature degree is 32～45 DEG C, and crystallizer magma temperature is low compared to cooler drop temperature 1～5 DEG C；
(3) magma crystal after centrifugal filtration is packed after continuous low temperature drying, and baking temperature is 50～60 DEG C.
2. continuous crystallisation technique as claimed in claim 1 it is characterised in that: external cooler pass through control circulating pump flow
Come control material temperature and degree of supersaturation with the flow of recirculated cooling water and temperature, recirculated cooling water self-loopa amount be 200～
300m3/ h, recirculated cooling water gives back to coolant-temperature gage and is 32 DEG C and 38 DEG C.
3. continuous crystallisation technique as claimed in claim 1 it is characterised in that: crystallizer by control agitator rotating speed control
Circulating load processed, so that crystal suspension.
4. continuous crystallisation technique as claimed in claim 1 it is characterised in that: crystallizer is provided with fine crystal elimination device, is used for
Supernatant containing a large amount of fine crystals is returned evaporization process dissolving, thus ensureing growing up of crystal in crystallizer, supernatant
Returning liquid measure is 0～3m3/h.
5. continuous crystallisation technique as claimed in claim 1 it is characterised in that: drying adopts vibrating distributor, and mother solution returns and steams
Send out operation.
6. technique as claimed in claim 1 it is characterised in that: described in step 1, nickel sulfate solution mass percent is preferably 38
～39%, cobalt sulfate solution mass percent is preferably 33～34%.
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| CN201410461339.1A CN104192917B (en) | 2014-09-06 | 2014-09-06 | Nickel-cobalt sulfate continuous-crystallizing process |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668651B (en) * | 2016-02-03 | 2017-03-22 | 广东佳纳能源科技有限公司 | Production method for cobaltous sulfate heptahydrate |
| CN105776705B (en) * | 2016-04-12 | 2018-10-23 | 衢州华友钴新材料有限公司 | A kind of cobalt nickel fibers waste water comprehensive resources treatment method |
| CN107381637B (en) * | 2017-09-04 | 2019-04-16 | 河钢股份有限公司承德分公司 | A kind of method of preventing scaring in ammonium metavanadate crystallization process |
| CN109173329B (en) * | 2018-10-31 | 2023-08-29 | 浙江新和成股份有限公司 | Device for evaporative crystallization |
| CN110665249A (en) * | 2019-10-24 | 2020-01-10 | 昆山三一环保科技有限公司 | MVR high-salinity wastewater crystallization and salt discharge system and process method thereof |
| CN111905398A (en) * | 2020-06-26 | 2020-11-10 | 中国轻工业长沙工程有限公司 | Process for producing nickel cobalt salt and ammonium salt by continuous crystallization |
| US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
| CN113476885A (en) * | 2021-07-08 | 2021-10-08 | 斯瑞尔环境科技股份有限公司 | Method for continuously producing iron salt crystals |
| CN113457200A (en) * | 2021-07-09 | 2021-10-01 | 西安航天华威化工生物工程有限公司 | Accurate path control continuous crystallization system for nickel sulfate |
| CN114534302B (en) * | 2022-03-21 | 2023-09-19 | 金川集团镍盐有限公司 | Method for continuously cooling and crystallizing nickel sulfate |
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| CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
| CN202983245U (en) * | 2012-11-22 | 2013-06-12 | 中节能六合天融环保科技有限公司 | MVR (Mechanical Vapor Recompression) evaporator applicable to concentration of magnesium sulfate solution |
| CN103172088A (en) * | 2013-04-11 | 2013-06-26 | 南风化工集团股份有限公司 | Application of MVR (mechanical vapor recompression) crystallizing evaporator in sodium sulfate and sodium chloride separation technology |
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| CN102040252A (en) * | 2009-10-16 | 2011-05-04 | 中科铜都粉体新材料股份有限公司 | Method for producing battery-level refined nickel sulfate with electrolyte |
| CN202983245U (en) * | 2012-11-22 | 2013-06-12 | 中节能六合天融环保科技有限公司 | MVR (Mechanical Vapor Recompression) evaporator applicable to concentration of magnesium sulfate solution |
| CN103172088A (en) * | 2013-04-11 | 2013-06-26 | 南风化工集团股份有限公司 | Application of MVR (mechanical vapor recompression) crystallizing evaporator in sodium sulfate and sodium chloride separation technology |
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