CN108467051A - Crystal separator and method in potassium chloride magma - Google Patents

Crystal separator and method in potassium chloride magma Download PDF

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Publication number
CN108467051A
CN108467051A CN201810507054.5A CN201810507054A CN108467051A CN 108467051 A CN108467051 A CN 108467051A CN 201810507054 A CN201810507054 A CN 201810507054A CN 108467051 A CN108467051 A CN 108467051A
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outlet
mother liquor
separator
magma
crystallizer
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CN201810507054.5A
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CN108467051B (en
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韩昕玘
刘晗月
刘志刚
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NANJING AMETHYST VINE ENERGY CONSERVATION TECHNOLOGY Co Ltd
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NANJING AMETHYST VINE ENERGY CONSERVATION TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/22Preparation in the form of granules, pieces, or other shaped products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D2009/0086Processes or apparatus therefor
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Cyclones (AREA)

Abstract

The invention discloses crystal separator and methods in a kind of potassium chloride magma, belong to evaporative crystallization field.The technique includes mainly the equipment such as crystallizer, heater, separator, the brilliant tank of storage, circulating pump, clear liquid pump, raw material pump, Chu Jingfa, densitometer, feed valve, dump valve.It is characterized in that:The present invention carries out pre-separation using separator to unqualified magma small particles crystal, the clear liquid obtained at the top of separator is recycled as circulating mother liquor, the magma with little particle crystal that separator bottom obtains enters the brilliant tank of storage, the brilliant liquid of storage is mixed into the clear mother liquor flowed out from crystallizer enter crystallizer together in the brilliant tank of storage, continue crystal growth, so cycle is until grow into qualified magma;The impact that entire potassium chloride developmental process avoids circulating pump is damaged, ensure that the integrality of potassium chloride, while capable of preferably controlling potassium chloride grain size number, improves potassium chloride crystalline rate and its purity.

Description

Crystal separator and method in potassium chloride magma
Technical field
The present invention devises crystal separator and method in a kind of potassium chloride magma, belongs to evaporative crystallization field.
Background technology
Potassium chloride evaporative crystallization is that Klorvess Liquid evaporation and concentration is made to reach supersaturation, to which the mistake of potassium chloride be precipitated Journey.Potassium chloride crystallizes precipitation from solution need to undergo 2 steps, be to generate the microcosmic crystal grain for being known as nucleus as knot first Brilliant core, followed by nuclei growth become the crystal grain of macroscopic view.According to crystalline rate mechanism, the factor for influencing grain size number is main There are the relative velocity, viscosity, surface tension etc. of solution.
Common potassium chloride evaporative crystallization technique industrial at present mainly has the method that floatation and other methods are combined And adding halogen method.In order to make the grain size number of potassium chloride meet industrial requirements, in recent years people mainly from mold structure, Agitator speed and the several aspects of process cycles amount are improved, but still without eliminate unqualified crystal by circulating pump into The unfavorable factor being broken during entering circulating mother liquor.Quickly centrifugation impact easily causes little particle crystal to be damaged, even Rupture seriously affects little particle growth process, eventually leads to crystalline rate decline, and crystal quality deteriorates.
How to protect little particle crystal not damaged, accurately control grain size number, further increase crystalline rate, is current Urgent problem to be solved.
Invention content
Cause potassium chloride grain size number not by the present invention is broken for existing unqualified crystal crystal after circulating pump It is easy to control, the problems such as crystalline rate is low, propose the potassium chloride magma that a kind of average grain diameter is larger, surface area is small, crystalline rate is high Middle crystal separator and method.
Crystal separator in a kind of potassium chloride magma, it is characterised in that:Including crystallizer, heater, separator, Chu Jing Tank, clear liquid pump, raw material pump, Chu Jingfa, densitometer, material liquid import, qualified magma outlet, indirect steam outlet, adds circulating pump Hot steam import, condensate outlet, feed valve, dump valve;Crystallizer includes circulating mother liquor import, stores brilliant liquid import, top steaming Vapor outlet, clear mother liquor outlet and bottom end taphole;Heater includes that hot side entrance, hot side outlet, cold side input port and cold side go out Mouthful;Separator includes mother liquor import, top mother liquor outlet and the outlet of bottom end magma;The brilliant tank of storage includes magma import, clear mother liquor Import and the brilliant liquid outlet of storage;Densitometer includes dense mother liquor import, qualified outlet and unqualified outlet;Material liquid import passes through raw material Valve and raw material pump are connected with separator mother liquor import, and separator top mother liquor outlet passes through circulating pump and heater cold side input port phase Even, heater cold side outlet port is connected with crystallizer circulating mother liquor import, crystallizer bottom end taphole and the dense mother liquor of densitometer into Mouth is connected, and the outlet of densitometer qualification, which is exported by dump valve with qualified magma, to be connected, and the unqualified outlet of densitometer and separator are female Liquid import is connected, and magma outlet in separator bottom end is connected by storing up the brilliant tank magma import of brilliant valve and storage, and the clear mother liquor of crystallizer goes out Mouth is connected with by clear liquid pump with the brilliant clear mother liquor import of tank of storage, and the brilliant liquid outlet of the brilliant tank storage of storage is connected with the brilliant liquid import of crystallizer storage, Crystallizer top steam (vapor) outlet is connected with indirect steam outlet;Heating steam inlet is connected with heater hot side entrance, heater Hot side outlet is connected with condensate outlet.
The working method of crystal separator in a kind of potassium chloride magma, which is characterized in that including following work Process:Steam is heated by heating steam inlet, heater is flowed by heater hot side import, after exchanging heat with circulating mother liquor Condensate outlet is discharged to by heater hot side outlet;Material liquid flows into technological process from material liquid import, is pumped into through raw material Separator;Heater cold side import is flowed into through circulating pump by the circulating mother liquor of separator top mother liquor outlet outflow, is steamed with heating It is flowed out by heater cold side outlet port after vapour heat exchange;Circulating mother liquor after heating flows into crystallizer by crystallizer circulating mother liquor import, Flash distillation is completed in crystallizer and cools to hypersaturated state precipitation potassium chloride, and indirect steam is by crystallizer top steam (vapor) outlet It is discharged to indirect steam outlet, dense mother liquor flows into densitometer by crystallizer bottom end taphole:When magma density is eligible, Dense mother liquor is discharged to qualified magma outlet from the outlet of densitometer qualification;When magma density is ineligible, dense mother liquor is from density Unqualified outlet discharge is counted, mother liquor is mixed into material liquid and enters separator:The circulating mother liquor gone out by separator sub-argument is from separation The mother liquor outlet discharge of device top, so recycles;The little particle crystal isolated by separator is by separator bottom end magma outlet stream Go out;Magma with little particle crystal enters the brilliant tank of storage, under the action of clear liquid pump, by what is flowed out from the clear mother liquor outlet of crystallizer Clear mother liquor is blended into the brilliant liquid of storage in the brilliant tank of storage with magma, and the storage crystalline substance liquid with little particle crystal stores brilliant liquid inlet flow from crystallizer Enter crystallizer, continues crystal growth, so recycle.
Crystal separating technology in a kind of potassium chloride magma, it is characterised in that:Indirect steam exports and heating steam Import can not be communicated directly, but being heated by compressor makes indirect steam outlet and heating steam inlet communicate.
Crystal separator in a kind of potassium chloride magma, it is characterised in that:Separator using cyclone separator or Dilatation separator.Separator liquid level is kept constant in cyclic process, and liquid level is controlled by the brilliant valve of storage.
Crystal separator in a kind of potassium chloride magma, it is characterised in that:The clear mother liquor outlet of crystallizer is located at molten Below liquid liquid level at 0.2-0.5m.
The present invention carries out pre-separation using separator to unqualified magma small particles crystal, is obtained at the top of separator clear Liquid is recycled as circulating mother liquor, and the magma with little particle crystal that separator bottom obtains enters the brilliant tank of storage, brilliant in storage The brilliant liquid of storage is mixed into the clear mother liquor flowed out from crystallizer in tank and enters crystallizer together, continue crystal growth, so cycle is straight To growing into qualified magma;The impact that entire potassium chloride developmental process avoids circulating pump is damaged, ensure that potassium chloride crystalline substance The integrality of body improves potassium chloride crystalline rate and its purity while capable of preferably controlling potassium chloride grain size number.
Description of the drawings
Crystal separating technology flow chart in a kind of potassium chloride magmas of Fig. 1;
Label title in Fig. 1:1. crystallizer, 2. heaters, 3. separators, the brilliant tank of 4. storages, 5. circulating pumps, 6. clear liquid pumps, 7. is former Material pump, the brilliant valve of 8. storages, 9. densitometers, 10. material liquid imports, 11. qualified magma outlets, the outlet of 12. indirect steams, 13. heating Steam inlet, 14. condensate outlets, 15. feed valves, 16. dump valves.
Specific implementation method
Fig. 1 is crystal separating technology flow in a kind of potassium chloride magma proposed by the present invention, illustrates the technique referring to Fig. 1 The course of work.
Steam is heated by heating steam inlet 13, heater 2 is flowed by 2 hot side import of heater, is sent out with circulating mother liquor Condensate outlet 14 is discharged to by 2 hot side outlet of heater after raw heat exchange;
Material liquid flows into technological process from material liquid import 10, and separator 3 is sent into through raw material pump 7;Gone out by 3 top mother liquor of separator The circulating mother liquor of mouth outflow flows into 2 cold side import of heater through circulating pump 5, is gone out by 2 cold side of heater with after heating steam heat-exchanging Mouth outflow;Circulating mother liquor after heating flows into crystallizer 1 by 1 circulating mother liquor import of crystallizer, and flash distillation drop is completed in crystallizer 1 Potassium chloride is precipitated to saturation state in temperature, and indirect steam is discharged to indirect steam outlet 12 by 1 top steam (vapor) outlet of crystallizer, Dense mother liquor flows into densitometer 9 by 1 bottom end taphole of crystallizer:When magma density is eligible, dense mother liquor is closed from densitometer 9 Lattice outlet is discharged to qualified magma outlet 11;When magma density is ineligible, dense mother liquor is arranged from 9 unqualified outlet of densitometer Go out, being mixed into mother liquor with material liquid enters separator 3:The circulating mother liquor gone out by 3 sub-argument of separator goes out from 3 top mother liquor of separator Mouth discharge, so recycles;The little particle crystal isolated by separator 3 is by 3 bottom end magma outlet outflow of separator;With small The magma of grain crystal enters the brilliant tank 4 of storage and is existed by the clear mother liquor flowed out from 1 clear mother liquor outlet of crystallizer under the action of clear liquid pump 6 The brilliant liquid of storage is blended into storage crystalline substance tank 4 with magma, the storage crystalline substance liquid with little particle crystal stores brilliant liquid import inflow crystallization from crystallizer 1 Device 1 continues crystal growth, so recycles.

Claims (5)

1. crystal separator in a kind of potassium chloride magma, it is characterised in that:
Including crystallizer(1), heater(2), separator(3), the brilliant tank of storage(4), circulating pump(5), clear liquid pump(6), raw material pump (7), Chu Jingfa(8), densitometer(9), material liquid import(10), qualified magma outlet(11), indirect steam outlet(12), heating Steam inlet(13), condensate outlet(14), feed valve(15), dump valve(16);
Crystallizer(1)Go out including circulating mother liquor import, the brilliant liquid import of storage, top steam (vapor) outlet, clear mother liquor outlet and bottom end solution Mouthful;Heater(2)Including hot side entrance, hot side outlet, cold side input port and cold side outlet port;Separator(3)Including mother liquor import, top Hold mother liquor outlet and the outlet of bottom end magma;The brilliant tank of storage(4)Including magma import, clear mother liquor import and store brilliant liquid outlet;Density Meter(9)Including dense mother liquor import, qualified outlet and unqualified outlet;
Material liquid import(10)Pass through feed valve(15)It is pumped with raw material(7)With separator(3)Mother liquor import is connected, separator(3) Top mother liquor outlet passes through circulating pump(5)With heater(2)Cold side input port is connected, heater(2)Cold side outlet port and crystallizer(1) Circulating mother liquor import is connected, crystallizer(1)Bottom end taphole and densitometer(9)Dense mother liquor import is connected, densitometer(9)It is qualified Outlet passes through dump valve(16)It is exported with qualified magma(11)It is connected, densitometer(9)Unqualified outlet and separator(3)Mother liquor into Mouth is connected;Separator(3)Bottom end magma outlet passes through Chu Jingfa(8)With the brilliant tank of storage(4)Magma import is connected, crystallizer(1) Clear mother liquor outlet and pass through clear liquid pump(6)With the brilliant tank of storage(4)Clear mother liquor import is connected, and stores up brilliant tank(4)Store brilliant liquid outlet and crystallization Device(1)It stores brilliant liquid import to be connected, crystallizer(1)Top steam (vapor) outlet is exported with indirect steam(12)It is connected;
Heat steam inlet(13)With heater(2)Hot side entrance is connected, heater(2)Hot side outlet and condensate outlet(14) It is connected.
2. crystal separator in potassium chloride magma according to claim 1, it is characterised in that:Indirect steam exports(12) With heating steam inlet(13)It does not communicate directly, but being heated by compressor makes indirect steam export(12)With heating steam into Mouthful(13)It communicates.
3. crystal separator in potassium chloride magma according to claim 1, it is characterised in that:Separator(3)Using rotation Wind separator or dilatation separator.
4. crystal separator in potassium chloride magma according to claim 1, it is characterised in that:Crystallizer(1)Clear mother liquor Outlet is located at below liquid level of solution at 0.2-0.5m.
5. the working method of crystal separator in a kind of potassium chloride magma according to claim 1, which is characterized in that packet Include the following course of work:
Steam is heated by heating steam inlet(13), by heater(2)Hot side import flows into heater(2), with circulating mother liquor By heater after exchanging heat(2)Hot side outlet is discharged to condensate outlet(14);
Material liquid is from material liquid import(10)Technological process is flowed into, is pumped through raw material(7)It is sent into separator(3);By separator(3)Top Hold the circulating mother liquor of mother liquor outlet outflow through circulating pump(5)Flow into heater(2)By adding after cold side import, with heating steam heat-exchanging Hot device(2)Cold side outlet port flows out;Circulating mother liquor after heating is by crystallizer(1)Circulating mother liquor import flows into crystallizer(1), tying Brilliant device(1)Interior completion flash distillation cools to hypersaturated state and potassium chloride is precipitated, and indirect steam is by crystallizer(1)Top steam goes out Mouth is discharged to indirect steam outlet(12), dense mother liquor is by crystallizer(1)Bottom end taphole flows into densitometer(9):When magma is close When spending eligible, dense mother liquor is from densitometer(9)Qualification outlet is discharged to qualified magma outlet(11);When magma density is not met When condition, dense mother liquor is from densitometer(9)Unqualified outlet discharge, is mixed into mother liquor with material liquid and enters separator(3):By detaching Device(3)The circulating mother liquor that sub-argument goes out is from separator(3)Top mother liquor outlet discharge, so recycles;By separator(3)It isolates Little particle crystal is by separator(3)Bottom end magma outlet outflow;Magma with little particle crystal enters the brilliant tank of storage(4), clear Liquid pump(6)Under the action of, by from crystallizer(1)The clear mother liquor of clear mother liquor outlet outflow is in the brilliant tank of storage(4)It is interior to be blended into magma Brilliant liquid is stored, the storage crystalline substance liquid with little particle crystal is from crystallizer(1)It stores brilliant liquid import and flows into crystallizer(1), continue crystal growth, So cycle.
CN201810507054.5A 2018-05-24 2018-05-24 Device and method for separating crystals in potassium chloride crystal slurry Active CN108467051B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111054294A (en) * 2020-01-13 2020-04-24 中国科学院青岛生物能源与过程研究所 Method for returning small crystal particles in discharged slurry of reactive crystallizer
CN114887347A (en) * 2022-05-23 2022-08-12 青岛科技大学 Method for extracting mature large crystal particles from crystallizer

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1429596A (en) * 1964-03-12 1966-02-25 Allied Chem Process for producing dense crystalline anhydrous sodium carbonate
US4160812A (en) * 1977-09-20 1979-07-10 Texasgulf Inc. Multi-stage crystallization of sodium carbonate
CN104843745A (en) * 2015-04-27 2015-08-19 青海国泰盐湖化肥有限公司 Control method for granularity of potassium nitrate product produced through double decomposition
US20150329369A1 (en) * 2014-05-19 2015-11-19 Carbon Engineering Limited Partnership Recovering a caustic solution via calcium carbonate crystal aggregates
CN205204845U (en) * 2015-11-23 2016-05-04 金川集团股份有限公司 Thin brilliant elimination and hierarchical recycling system of sodium hydrosulphite parting liquid
CN106693414A (en) * 2017-01-06 2017-05-24 南京航空航天大学 Heat-mass co-transfer evaporation and crystallization system and working method thereof
CN208617377U (en) * 2018-05-24 2019-03-19 南京紫晶藤节能科技有限公司 Crystal separator in potassium chloride magma

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1429596A (en) * 1964-03-12 1966-02-25 Allied Chem Process for producing dense crystalline anhydrous sodium carbonate
US4160812A (en) * 1977-09-20 1979-07-10 Texasgulf Inc. Multi-stage crystallization of sodium carbonate
US20150329369A1 (en) * 2014-05-19 2015-11-19 Carbon Engineering Limited Partnership Recovering a caustic solution via calcium carbonate crystal aggregates
CN104843745A (en) * 2015-04-27 2015-08-19 青海国泰盐湖化肥有限公司 Control method for granularity of potassium nitrate product produced through double decomposition
CN205204845U (en) * 2015-11-23 2016-05-04 金川集团股份有限公司 Thin brilliant elimination and hierarchical recycling system of sodium hydrosulphite parting liquid
CN106693414A (en) * 2017-01-06 2017-05-24 南京航空航天大学 Heat-mass co-transfer evaporation and crystallization system and working method thereof
CN208617377U (en) * 2018-05-24 2019-03-19 南京紫晶藤节能科技有限公司 Crystal separator in potassium chloride magma

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111054294A (en) * 2020-01-13 2020-04-24 中国科学院青岛生物能源与过程研究所 Method for returning small crystal particles in discharged slurry of reactive crystallizer
CN114887347A (en) * 2022-05-23 2022-08-12 青岛科技大学 Method for extracting mature large crystal particles from crystallizer
CN114887347B (en) * 2022-05-23 2023-11-17 青岛科技大学 Method for extracting mature large crystal particles from crystallizer

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