CN108939601A - A method of cobalt chloride is prepared by cobalt chloride solution evaporative crystallization - Google Patents
A method of cobalt chloride is prepared by cobalt chloride solution evaporative crystallization Download PDFInfo
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- CN108939601A CN108939601A CN201810918886.6A CN201810918886A CN108939601A CN 108939601 A CN108939601 A CN 108939601A CN 201810918886 A CN201810918886 A CN 201810918886A CN 108939601 A CN108939601 A CN 108939601A
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- cobalt chloride
- evaporation
- falling film
- chloride solution
- heat
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- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 title claims abstract description 91
- 238000002425 crystallisation Methods 0.000 title claims abstract description 46
- 230000008025 crystallization Effects 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000001704 evaporation Methods 0.000 claims abstract description 76
- 230000008020 evaporation Effects 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000243 solution Substances 0.000 claims abstract description 53
- 239000012452 mother liquor Substances 0.000 claims abstract description 29
- 239000012047 saturated solution Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000011552 falling film Substances 0.000 claims description 57
- 239000002994 raw material Substances 0.000 claims description 40
- 230000005484 gravity Effects 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 11
- 239000002360 explosive Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 230000009977 dual effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000009835 boiling Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000007689 inspection Methods 0.000 description 5
- 238000005070 sampling Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005373 pervaporation Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000004872 foam stabilizing agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/08—Halides
- C01G51/085—Chlorides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention belongs to the preparation technical field of cobalt chloride, in particular to a kind of method that cobalt chloride is prepared by cobalt chloride solution evaporative crystallization.Free water of the cobalt chloride in addition to the crystallization water is all evaporated in evaporation stage, mother liquor is avoided and needs duplicate heating, cooling process.It is followed and is evaporated using two compressor sections in series methods or direct two, solve the problems, such as that the boiling point heating of solution is higher；In crystallization process, the super dense cobalt chloride solution for completely removing free water is added in cold cobalt chloride saturated solution, so that the degree of supersaturation of cobalt chloride is effectively controlled, so that production can carry out, and obtains the very big crystallization of particle.
Description
Technical field
The invention belongs to the preparation technical field of cobalt chloride, in particular to one kind prepares chlorine by cobalt chloride solution evaporative crystallization
Change the method for cobalt.
Background technique
Existing salting liquid method of evaporating be using single-action autoclave evaporate, energy consumption is big, evaporation to a certain extent i.e. into
Row crystallisation by cooling, the mother liquor after crystallization continue back to be evaporated in kettle, and the mother liquor in system, which is repeated, to be heated, is cooled down, again
Heating, energy loss are very big.
The main application of cobalt chloride are as follows: be used as production barometer, densimeter, dry and wet indicator etc., pottery in instrument manufacturing
Porcelain industry is used as colorant, and coatings industry is used to prepare mixed feed, brewery industry in animal husbandry for manufacturing paint drier
As Beer Foam Stabilizers, national defense industry is used as catalyst, is used in analytical chemistry for manufacturing poison gas cover in chemical reaction
Spot analysis zinc, haploid breeding, in addition, being also used to manufacture invisible ink, paper of cobalt chloride,test, discoloration silica gel etc. also serves as ammonia
Absorbent.
Cobalt chloride crystal is stable at room temperature, and the crystallization water is lost after heated and becomes blue, is then become again in wet air
Return red.Existing cobalt chloride solution uses autoclave atmospheric evaporation, crystallisation by cooling, and mother liquor, which returns kettle, to be continued to evaporate, and crystallization obtains chlorination
Yield of cobalt is 28%, density 1.52g/mL, the disadvantages of the method are as follows process flow is long, energy consumption is high, and due to a large amount of mother liquors
Cooling heating causes operating cost high, and equipment investment is more, and the chlorination cobalt granule crystallized is too small, need to be using band filter cloth formula interval
Centrifuge, efficiency are extremely low.
Summary of the invention
The present invention provides a kind of crystal grain is larger, crystallizes and lower-cost chlorine is prepared by cobalt chloride solution evaporative crystallization
Change the method for cobalt.
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, by enter after raw material pump pressurization 1 grade of heat exchanger into
Row preheating, then after 2 grades of preheaters preheat, into falling film evaporator；
Wherein, as used double-effect evaporation, stoste enters 1 grade of heat exchanger after raw material pump pressurization and is preheating to 60-65 DEG C, then
It is heated to 75-80 DEG C through 2 grades of preheaters, is entered back into falling film evaporator；
It is such as evaporated using MVR, stoste enters 1 grade of heat exchanger after raw material pump pressurization and is preheating to 45-50 DEG C, then through 2 grades
Preheater is heated to 60-65 DEG C, enters back into falling film evaporator；
The temperature of preheating is that the temperature needed by its final evaporation determines that the temperature that MVR finally evaporates is low, be it requires
The temperature of preheating is also low, and double-effect evaporation temperature is high, and the temperature for needing to preheat is also high.
(2) it is concentrated by evaporation:
Falling film evaporation: the cobalt chloride solution that step (1) preheats is pumped into falling film evaporator, the original in falling film evaporator pipe
Material is pumped into forcing vaporiser after being concentrated raw material explosive evaporation, raw material with pipe external heat steam heat-exchanging；Falling film evaporation can
Think economic benefits and social benefits falling film evaporation or MVR evaporation；Wherein, then the evaporation of two effects is first carried out again using economic benefits and social benefits falling film evaporation cobalt chloride solution
Carry out an effect evaporation；Level-one evaporation is first carried out using MVR evaporation cobalt chloride solution and carries out dual evaporation again.
MVR evaporation uses the evaporation mode of sequence, and material uses the evaporation mode of backward, object by level-one to second level, economic benefits and social benefits
Material enough guarantees that the temperature of concentrated solution is greater than 86 DEG C to an efficiency by two effects, and material can be dissolved in the crystallization water of its own.
Forced evaporation: the heat exchanger shell of forcing vaporiser is passed through live steam, make raw material in forcing vaporiser pipe with
Shell steam heat-exchanging evaporates raw material, is concentrated after the concentration of cobalt chloride reaches 54-55%, is continuously introduced into again by potential difference
In gravity tank；
The concentration of cobalt chloride is directly increased to 54-55% by evaporation stage, i.e., by cobalt chloride solution in addition to the crystallization water
Free water all evaporate, since temperature is more than 85 DEG C after the completion of evaporation, cobalt chloride is dissolved in the crystallization water of its own,
Basic or solution state avoids the process that mother liquor needs duplicate heating, cooling, heats up again, and will can disposably produce
Product cobalt chloride whole evaporative crystallization comes out.
Wherein, the secondary steam generated through double-effect evaporation returns to heat source of the preheater as preheater, falling film evaporator
The condensed water that heat exchanger generates enters condensate water pot after the bottom of heat exchanger is collected；
The secondary steam that forcing vaporiser generates enters falling film evaporation after separator is the drop separation in water vapour
Device shell；The condensed water that the heat exchanger of forcing vaporiser generates enters condensate water pot after the bottom of heat exchanger is collected.
The free water pervaporation in cobalt chloride solution in addition to the crystallization water is come out in evaporation process, so that primary receive
Rate greatly improves, and processing cost is greatly reduced, which makes the elevation of boiling point of solution higher, reaches 21 degree, using multiple-effect method
It is feasible for being evaporated.
The secondary steam generated through MVR evaporation is entered respective separator to separate the drop in vapor from steam
Go out to form secondary steam, secondary steam enters centrifugal compressor, after vapor is compressed temperature and pressure increase, a part into
Enter falling film evaporator shell heated material, the vapor of another part higher temperature enters lobed rotor compressor, further increases temperature
Enter outside forcing vaporiser heat exchanger tube after degree and pressure, exchange heat with raw material in pipe, vapor releases latent heat and is condensed into condensation
Water.
The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters Falling film heat transfer device shell, the heat exchange of falling film evaporator
The condensed water that device generates enters condensate water pot after the bottom of heat exchanger is collected.
The free water pervaporation in cobalt chloride solution in addition to the crystallization water is come out in evaporation process, so that solution
The elevation of boiling point is higher, reaches 21 degree, far more than the ability of usual MVR evaporator, therefore solves temperature using the series connection of two compressors
The problem of raising, centrifugal compressor and lobed rotor compressor, completely series connection can also be realized with sections in series, it is contemplated that pressure
The processing capacity level-one cost of investment of contracting machine, the present invention is practical to be realized using centrifugation and the sections in series method of Roots.
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and crystalline particle is obtained；
Free water all evaporate during since the degree of supersaturation of cobalt chloride is higher, be decreased slightly as temperature may form one
Temperature cannot be greater than 85 DEG C by the direct crystallisation by cooling of liquid of so high degree of supersaturation, therefore, in crystallization process by block
The super dense cobalt chloride solution of removal free water, which is added in cold cobalt chloride saturated solution, (it is female to can be the separation originally crystallized
Liquid is also possible to the cobalt chloride saturated solution newly configured, and only needing for newly configuring is primary, later can reuse always), so that chlorine
Change cobalt degree of supersaturation be effectively controlled, thus solve free water is all evaporated during due to cobalt chloride mistake
Saturation degree is higher, is decreased slightly as the problem of temperature may form one piece, so that production can carry out, and obtains the very big knot of particle
It is brilliant.
Wherein, the quality of cold cobalt chloride saturated solution is 1 times -5 times of the quality of super dense cobalt chloride solution preferable.
(4) be centrifugated: crystalline particle continuously enters centrifuge, is centrifuged, and mother liquor enters mother liquor tank, using mother
Liquid pump is by mother liquor blowback high position crystallizing tank；
(5) it packs: the solids package after centrifuge separation.
Condensing cooler, regulating valve, steam-water separator, vacuum pump group do not guarantee that evaporator operation is being set at voltage-stabilizing system
Pressure is counted, to guarantee that evaporating temperature is stablized in technique claimed range.
The utility model has the advantages that
The present invention comes out the free water pervaporation in cobalt chloride solution in addition to the crystallization water in evaporation process, avoids
Mother liquor needs duplicate heating, cooling processes.It is followed and is steamed using two compressor sections in series methods or direct two
Hair solves the problems, such as that the boiling point heating of solution is higher；In crystallization process, the super dense cobalt chloride of free water will be completely removed
Solution is added in cold cobalt chloride saturated solution, so that and the degree of supersaturation of cobalt chloride is effectively controlled, so that
Production can carry out, and obtain the very big crystallization of particle.
Evaporation technology of the present invention is more more energy efficient than existing evaporation technology, and saving energy 60% is more more stable than existing evaporation technology.?
Advantageous crystalline body is arrived.
Detailed description of the invention
Fig. 1 is the process flow chart of the embodiment of the present invention 1；
Fig. 2 is the process flow chart of the embodiment of the present invention 2；
Fig. 3 is the crystallization figure for the cobalt chloride that the embodiment of the present invention 1 obtains；
Fig. 4 is the crystallization figure for the cobalt chloride that comparative example 1 of the present invention obtains.
Specific embodiment
Below by specific embodiment, the present invention will be described in detail.
Embodiment 1
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, by entering 1 grade of plate-type heat-exchange after raw material pump pressurization
Device is preheating to 65 DEG C, is then heated to 77 DEG C through 2 grades of preheaters, enters back into falling film evaporator；
(2) it is concentrated by evaporation:
Falling film evaporation: the cobalt chloride solution that step (1) preheats is pumped into two effect falling film evaporators, in falling film evaporator pipe
Raw material and pipe external heat steam heat-exchanging make raw material explosive evaporation, be then fed into an effect falling film evaporator, falling film evaporator pipe
Interior raw material and pipe external heat steam heat-exchanging is pumped into forcing vaporiser after being concentrated raw material explosive evaporation, raw material；
Forced evaporation: the heat exchanger shell of forcing vaporiser is passed through live steam, make raw material in forcing vaporiser pipe with
Shell steam heat-exchanging evaporates raw material, is concentrated after the concentration of cobalt chloride reaches 54-55%, is continuously introduced into again by potential difference
In gravity tank；
Wherein, the secondary steam that falling film evaporator evaporation generates returns to heat source of the preheater as preheater, falling film evaporation
The condensed water that the heat exchanger of device generates enters condensate water pot after the bottom of heat exchanger is collected；Again be concentrated until cobalt chloride it is dense
After degree reaches 54-55%, it is continuously introduced into gravity tank by potential difference.
The secondary steam that forcing vaporiser generates enters falling film evaporation after separator is the drop separation in water vapour
Device shell；The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters condensate water pot after the bottom of heat exchanger is collected.
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and crystalline particle is obtained；
In crystallization process, the super dense cobalt chloride solution that temperature is greater than 85 DEG C of basic removal free waters is added to cold
Make the degree of supersaturation of cobalt chloride be effectively controlled in cobalt chloride saturated solution, so that production can carry out, obtains
The very big crystallization of grain, wherein the quality of cold cobalt chloride saturated solution is 1.5 times of the quality of super dense cobalt chloride solution.
(4) be centrifugated: crystalline particle continuously enters centrifuge, is centrifuged, and mother liquor enters mother liquor tank, mother liquor pump
By mother liquor blowback high position crystallizing tank；
(5) it packs: the solids package after centrifuge separation.
Feedstock solution: salt content about 34%, density 1.34g/mL, PH > 1, inlet amount: 11.123T/h, 4.2 tons of evaporation capacity/
Hour, the saturated solution elevation of boiling point :≤22 DEG C, power consumption of compressor :≤73Kwh/T, discharge states of matter: CoCL2 6H2O, distilled water
It is limpid, PH > 3.2；
Sampling inspection results: partial size 1.5-2mm.
Embodiment 2
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, by entering 1 grade of plate-type heat-exchange after raw material pump pressurization
Device is preheating to 48 DEG C, is then heated to 65 DEG C through 2 grades of preheaters, enters back into falling film evaporator；
(2) it is concentrated by evaporation:
Falling film evaporation: the cobalt chloride solution that step (1) preheats is pumped into MVR falling film evaporator, in falling film evaporator pipe
Raw material and pipe external heat steam heat-exchanging be concentrated raw material explosive evaporation, raw material after be pumped into forcing vaporiser；
Forced evaporation: the heat exchanger shell of forcing vaporiser is passed through live steam, make raw material in forcing vaporiser pipe with
Shell steam heat-exchanging evaporates raw material, is concentrated after the concentration of cobalt chloride reaches 54-55%, is continuously introduced into again by potential difference
In gravity tank；
Wherein, enter respective separator into the secondary steam that falling film evaporator and forcing vaporiser are evaporated generation
Drop in vapor is separated to form secondary steam from steam, secondary steam enters centrifugal compressor, vapor quilt
Temperature and pressure increases after compression, and a part enters falling film evaporator shell heated material, and the water of another part higher temperature steams
Gas enters lobed rotor compressor, enters outside forcing vaporiser heat exchanger tube after further increasing temperature and pressure, changes with raw material in pipe
Heat, vapor release latent heat and are condensed into condensed water.
The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters Falling film heat transfer device shell, the heat exchange of falling film evaporator
The condensed water that device generates enters condensate water pot after the bottom of heat exchanger is collected.
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and crystalline particle is obtained；
In crystallization process, the super dense cobalt chloride solution for removing free water is added to cold cobalt chloride saturated solution
In, so that the degree of supersaturation of cobalt chloride is effectively controlled, so that production can carry out, it is very big to obtain particle
Crystallization, wherein the quality of cold cobalt chloride saturated solution is 3 times of the quality of super dense cobalt chloride solution.
(4) be centrifugated: crystalline particle continuously enters centrifuge, is centrifuged, and mother liquor enters mother liquor tank, mother liquor pump
By mother liquor blowback high position crystallizing tank；
(5) it packs: the solids package after centrifuge separation.
Feedstock solution: salt content about 34%, density 1.34g/mL, PH > 1.5, inlet amount: 11.123T/h, evaporation capacity 4.2
Ton/hour, the saturated solution elevation of boiling point :≤22 DEG C, power consumption of compressor :≤73Kwh/T, discharge states of matter: CoCL2 6H2O, distillation
Water is limpid, PH > 3.2；
Sampling inspection results: partial size 1-2mm.
Embodiment 3
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, by entering 1 grade of plate-type heat-exchange after raw material pump pressurization
Device is preheating to 60 DEG C, is then heated to 75 DEG C through 2 grades of preheaters, enters back into falling film evaporator；
(3) crystallisation by cooling
In crystallization process, the super dense cobalt chloride solution for removing free water is added to cold cobalt chloride saturated solution
In, so that the degree of supersaturation of cobalt chloride is effectively controlled, so that production can carry out, it is very big to obtain particle
Crystallization, wherein the quality of cold cobalt chloride saturated solution is 5 times of the quality of super dense cobalt chloride solution.
Other steps are the same as embodiment 1.
Feedstock solution: salt content about 34%, density 1.34g/mL, PH > 1.5, inlet amount: 11.123T/h, evaporation capacity 4.2
Ton/hour, the saturated solution elevation of boiling point :≤22 DEG C, power consumption of compressor :≤73Kwh/T, discharge states of matter: CoCL2 6H2O, distillation
Water is limpid, PH > 3.2；
Sampling inspection results: partial size 1-2mm.
Comparative example 1
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, by entering 1 grade of plate-type heat-exchange after raw material pump pressurization
Device is preheating to 65 DEG C, is then heated to 77 DEG C through 2 grades of preheaters, enters back into falling film evaporator；
(2) it is concentrated by evaporation:
Falling film evaporation: the cobalt chloride solution that step (1) preheats is pumped into single-action falling film evaporator, single-action falling film evaporator
Raw material and pipe external heat steam heat-exchanging in pipe make raw material explosive evaporation；It is continuously introduced into gravity tank after concentration by potential difference；
Wherein, the secondary steam that falling film evaporator evaporation generates enters condenser condensation, and the heat exchanger of falling film evaporator produces
Raw condensed water enters condensate water pot after the bottom of heat exchanger is collected；
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and obtains crystalline particle, and mother liquor returns kettle evaporation.
(4) be centrifugated: crystalline particle continuously enters discontinuous centrifuge, is centrifuged, and mother liquor enters mother liquor tank, female
Liquid pump is by mother liquor blowback high position crystallizing tank；
(5) it packs: the solids package after centrifuge separation.
Sampling inspection results: partial size 0.15-0.2mm.
Comparative example 2
(1) it preheats:
The cobalt chloride solution of temperature >=30 DEG C is pumped into original fluid container, by entering 1 grade of plate-type heat-exchange after raw material pump pressurization
Device is preheating to 65 DEG C, is then heated to 77 DEG C through 2 grades of preheaters, enters back into falling film evaporator；
(2) it is concentrated by evaporation:
Falling film evaporation: the cobalt chloride solution that step (1) preheats is pumped into an effect falling film evaporator, an effect falling film evaporator
Raw material and pipe external heat steam heat-exchanging in pipe are pumped into forcing vaporiser after being concentrated raw material explosive evaporation, raw material；
Forced evaporation: the heat exchanger shell of forcing vaporiser is passed through live steam, make raw material in forcing vaporiser pipe with
Shell steam heat-exchanging evaporates raw material, is concentrated after the concentration of cobalt chloride reaches 54-55%, is continuously introduced into again by potential difference
In gravity tank；
Wherein, the secondary steam that falling film evaporator evaporation generates enters condenser condensation, and the heat exchanger of falling film evaporator produces
Raw condensed water enters condensate water pot after the bottom of heat exchanger is collected；
The secondary steam that forcing vaporiser generates enters falling film evaporation after separator is the drop separation in water vapour
Device shell；The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters condensate water pot after the bottom of heat exchanger is collected.
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and crystalline particle is obtained；
(4) be centrifugated: crystalline particle continuously enters centrifuge, is centrifuged, and mother liquor enters mother liquor tank, mother liquor pump
By mother liquor blowback high position crystallizing tank；
(5) it packs: the solids package after centrifuge separation.Sampling inspection results: partial size 0.2-0.3mm.
Claims (6)
1. a kind of method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization, it is characterised in that: the method comprises the following steps:
(1) it preheats:
The cobalt chloride solution of temperature >=10 DEG C is pumped into original fluid container, is carried out in advance by entering 1 grade of heat exchanger after raw material pump pressurization
Heat, then after 2 grades of preheaters preheat, into falling film evaporator；
(2) it is concentrated by evaporation:
Falling film evaporation: by step (1) preheat cobalt chloride solution be pumped into falling film evaporator, the raw material in falling film evaporator pipe with
Pipe external heat steam heat-exchanging is pumped into forcing vaporiser after being concentrated raw material explosive evaporation, raw material；Wherein, falling film evaporation is
Economic benefits and social benefits falling film evaporation or MVR evaporation；Wherein, the evaporation of two effects is first carried out using economic benefits and social benefits falling film evaporation cobalt chloride solution then to carry out again
One effect evaporation；Level-one evaporation is first carried out using MVR evaporation cobalt chloride solution and carries out dual evaporation again；
Forced evaporation: forcing vaporiser heat exchanger shell is passed through live steam, steams raw material and shell in forcing vaporiser pipe
Vapour heat exchange evaporates raw material, after being concentrated to design density again, is continuously introduced into gravity tank by potential difference；
(3) crystallisation by cooling: the concentrate that will be fed into gravity tank is crystallized, and crystalline particle is obtained；
(4) be centrifugated: crystalline particle continuously enters centrifuge, is centrifuged, and mother liquor enters mother liquor tank, and mother liquor pump will be female
Liquid pump returns high-order crystallizing tank；
(5) it packs: the solids package after centrifuge separation.
2. the method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization as described in claim 1, it is characterised in that: using double
The temperature that effect evaporates into the preheating of 1 grade of heat exchanger is 60-65 DEG C, is then heated to 75-80 DEG C through 2 grades of preheaters；It is steamed using MVR
Hair enters 1 grade of heat exchanger and is preheating to 45-50 DEG C, is then heated to 60-65 DEG C through 2 grades of preheaters.
3. the method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization as described in claim 1, it is characterised in that: using double
The secondary steam that effect evaporation generates returns to heat source of the preheater as preheater, the condensed water that the heat exchanger of falling film evaporator generates
Enter condensate water pot after the bottom of heat exchanger is collected；
The secondary steam that forcing vaporiser generates enters falling film evaporator shell after separator is the drop separation in water vapour
Layer；The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters condensate water pot after the bottom of heat exchanger is collected.
4. the method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization as described in claim 1, it is characterised in that: use
MVR evaporation generate secondary steam enter respective separator the drop in vapor is separated from steam to be formed it is secondary
Steam, secondary steam enter centrifugal compressor, and temperature and pressure increases after vapor is compressed, and a part enters falling film evaporator
The vapor of shell heated material, another part higher temperature enters lobed rotor compressor, and it is laggard to further increase temperature and pressure
Enter outside forcing vaporiser heat exchanger tube, exchange heat with raw material in pipe, vapor releases latent heat and is condensed into condensed water；
The condensed water that the forced heat-exchanging device of forcing vaporiser generates enters Falling film heat transfer device shell, and the heat exchanger of falling film evaporator produces
Raw condensed water enters condensate water pot after the bottom of heat exchanger is collected.
5. the method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization as described in claim 1, it is characterised in that: condensation knot
During crystalline substance, the super dense cobalt chloride solution for removing free water is added in cold cobalt chloride saturated solution and is crystallized.
6. the method for preparing cobalt chloride by cobalt chloride solution evaporative crystallization as claimed in claim 5, it is characterised in that: cold chlorine
Change the mother liquor that cobalt saturated solution is Crystallization Separation, or the cobalt chloride saturated solution newly configured, cold cobalt chloride saturated solution is added
Quality be 1-5 times of quality of super dense cobalt chloride solution.
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