CN217627643U - Lithium hydroxide conversion solution continuous Miscanthus removal production process system - Google Patents

Lithium hydroxide conversion solution continuous Miscanthus removal production process system Download PDF

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CN217627643U
CN217627643U CN202221406065.2U CN202221406065U CN217627643U CN 217627643 U CN217627643 U CN 217627643U CN 202221406065 U CN202221406065 U CN 202221406065U CN 217627643 U CN217627643 U CN 217627643U
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primary
freezing
mother liquor
pump
heat exchanger
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赵拓
李敏
张小江
周齐
陈竹林
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Jiangsu Sunevar Energy Technology Co ltd
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Jiangsu Sunevar Energy Technology Co ltd
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The utility model provides a lithium hydroxide conversion solution continuous Miscanthus nites-removing production process system, which comprises a feeding tank, a feeding pump, a precooler, a primary freezing heat exchanger, a primary freezing crystallizer, a primary freezing discharge pump, a primary freezing thickener, a primary centrifuge, a primary mother liquor tank and a primary mother liquor pump which are connected in sequence; the secondary refrigeration heat exchanger, the secondary refrigeration crystallizer, the secondary refrigeration discharge pump, the secondary refrigeration thickener, the secondary centrifuge, the secondary mother liquor tank, the secondary mother liquor pump and the precision filter are connected in sequence; the two-stage freezing crystallization mirabilite separated by the two-stage centrifuge and the conversion liquid of the former process enter a feeding tank together to be used as the stock solution of the one-stage freezing crystallization; the mother liquor of being separated by second grade centrifuge then passes through second grade mother liquor jar, second grade mother liquor pump, gets into discharge system behind precision filter separation mirabilite fine grain reentrant precooler and stoste heat transfer, the utility model discloses the lithium hydroxide of smuggleing secretly is few, and stability and treatment effeciency are all higher.

Description

Lithium hydroxide conversion solution continuous Miscanthus removal production process system
Technical Field
The utility model relates to a denitration production process system, in particular to a lithium hydroxide conversion solution continuous denitration production process system.
Background
At present, mirabilite in the conventional lithium hydroxide conversion solution removing solution is mostly separated out by adopting a reaction kettle cooler or a primary circulation freezing mode, and the problems of small treatment amount, more lithium hydroxide entrained in crystallized mirabilite and the like exist by adopting the existing method.
The patent lithium hydroxide mirabilite continuous freezing crystallization device (with the publication number of CN 208711098U) has the advantages of stable continuous production operation, large scale, capability of relieving frequent equipment blockage and prolonging the cleaning period of the equipment, and simultaneously, a plurality of methods for cleaning the equipment without stopping on line can be provided, but a discharge port of a first crystallizer in the device is connected with a feed port of a second crystallizer, so that a product is obtained by crystallizing a primary crystal after the primary crystal is mixed into a secondary crystal, and the problem that the crystal carries more impurities exists;
therefore, a production process system for continuously removing Mirabilitum from lithium hydroxide conversion solution, which has the advantages of large crystallized mirabilite particles, low water content, less entrained lithium hydroxide and higher stability and treatment efficiency, is urgently needed.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a lithium hydroxide conversion liquid takes off mirabilite production technology system in succession, and the glauber's salt granule that crystallizes out is big, and the water content is low to the lithium hydroxide of smuggleing secretly is few, and stability and treatment effeciency are all higher.
The utility model provides a following technical scheme:
a production process system for continuously removing Miscanthus sodium from a lithium hydroxide conversion solution comprises a primary freezing unit and a secondary freezing unit;
the primary refrigeration unit comprises a feeding tank, a feeding pump, a precooler, a primary refrigeration heat exchanger, a primary refrigeration crystallizer, a primary refrigeration discharge pump, a primary refrigeration thickener, a primary centrifuge, a primary mother liquor tank and a primary mother liquor pump which are connected in sequence;
the secondary refrigeration unit comprises a secondary refrigeration heat exchanger, a secondary refrigeration crystallizer, a secondary refrigeration discharge pump, a secondary refrigeration thickener, a secondary centrifuge, a secondary mother liquor tank, a secondary mother liquor pump and a precision filter which are connected in sequence;
after the primary centrifuge centrifugally separates the entering crystal slurry, the solid mirabilite is discharged out of the system as a product, and the mother liquor enters a primary mother liquor tank; the primary refrigeration mother liquor enters a secondary refrigeration circulating pipeline through a primary mother liquor pump, and feed liquid enters a tube side of a secondary refrigeration heat exchanger to exchange heat with a refrigerant of a shell side under the pushing of a secondary refrigeration circulating pump;
the two-stage freezing crystallization mirabilite separated by the two-stage centrifuge and the conversion liquid of the former process enter a feeding tank together to be used as the stock solution of the one-stage freezing crystallization; the mother liquor separated by the secondary centrifuge enters a precision filter through a secondary mother liquor tank and a secondary mother liquor pump to separate mirabilite fine crystals, and then enters a precooler to exchange heat with the stock solution and then is discharged out of the system.
Preferably, the circulation of the feed liquid is realized between the primary refrigeration heat exchanger and the primary refrigeration crystallizer through a primary refrigeration circulating pump, the feed liquid enters a tube side of the primary refrigeration heat exchanger to exchange heat with a refrigerant of a shell side, and the feed liquid enters the primary refrigeration crystallizer for crystallization after being cooled.
Preferably, the refrigerant on the shell side of the first-stage refrigeration heat exchanger circulates in a large amount under the action of a first-stage refrigerant circulating pump, and is connected with the refrigerator through a first-stage refrigerant pump to supplement the low-temperature refrigerant to maintain the temperature difference between the inside and the outside of the heat exchange pipe of the first-stage refrigeration heat exchanger.
Preferably, the temperature in the primary freezing crystallizer is controlled at 5 ℃, the shell side temperature of the primary freezing heat exchanger is controlled at 0 ℃, the solid content of the feed slurry of the primary centrifuge is controlled at 40%, and the primary centrifuge adopts a piston double-push centrifuge.
Preferably, the circulation of the feed liquid is realized between the secondary refrigeration heat exchanger and the secondary refrigeration crystallizer through a secondary refrigeration circulating pump, the feed liquid enters a tube side of the secondary refrigeration heat exchanger to exchange heat with the refrigerant of a shell side, and the feed liquid enters the secondary refrigeration crystallizer for crystallization after being cooled.
Preferably, the refrigerant on the shell side of the secondary refrigeration heat exchanger is largely circulated under the action of a secondary refrigerant circulating pump, and is connected with the refrigerator through the secondary refrigerant pump to supplement the low-temperature refrigerant and maintain the temperature difference between the inside and the outside of the heat exchange pipe of the secondary refrigeration heat exchanger.
Preferably, the temperature in the secondary freezing crystallizer is controlled at minus 7 ℃, the shell side temperature of the secondary freezing heat exchanger is controlled at minus 12 ℃, the solid content of the feed slurry of the secondary centrifuge is controlled at 35 percent, and the secondary centrifuge adopts a spiral sedimentation filtration centrifuge.
The beneficial effects of the utility model are that: the utility model discloses be different from prior art, be according to the principle that the glauber's salt solubility reduces along with the reduction of temperature, whole technology adopts the two-stage freezing method, and wherein the freezing temperature of second grade is less than the one-level freezing, and the one-level freezing difference in temperature is little, and solution volume is big, and the glauber's salt granule of consequently crystallizing out is big, and the water content is low to the lithium hydroxide of smuggleing secretly is few, and the glauber's salt of crystallization can produce anhydrous sodium sulphate. The freezing mother liquor of one-level removes the further freezing glauber's salt that separates out of second grade, has taken out a large amount of water because of the glauber's salt is separated out, leads to lithium hydroxide content in the solution to improve, and the glauber's salt granule of crystallization is less relatively, and the moisture content is higher after centrifugal separation, and for reducing the lithium hydroxide loss, the glauber's salt that the second grade crystallization produced removes the feed tank and dissolves the recrystallization, and the second grade mother liquor has taken off most glauber's salt, can regard as lithium hydroxide crystallization raw materials, just the utility model discloses in only have the output product of one-level, the crystal that contains many magazines of second grade then returns the stoste of foremost and dissolves the refeeding.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention, and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic view of the construction of a portion of the primary refrigeration unit;
FIG. 3 is a schematic structural view of a portion of a secondary refrigeration unit;
Detailed Description
With reference to fig. 1 to 3, in this embodiment, the apparatus of the system includes a refrigerating machine 1, a feeding tank 2, a feeding pump 3, a pre-cooler 4, a primary refrigerant pump 5, a primary refrigerant circulating pump 6, a primary refrigerating heat exchanger 7, a primary refrigerating circulating pump 8, a primary freezing crystallizer 9, a primary freezing discharge pump 10, a primary freezing thickener 11, a primary centrifuge 12, a primary mother liquor tank 13, a primary mother liquor pump 14, a secondary refrigerant pump 15, a secondary refrigerant circulating pump 16, a secondary freezing heat exchanger 17, a secondary freezing circulating pump 18, a secondary freezing crystallizer 19, a secondary freezing discharge pump 20, a secondary freezing thickener 21, a secondary centrifuge 22, a secondary mother liquor tank 23, a secondary mother liquor pump 24, and a precision filter 25;
the specific process comprises the following steps:
a first-stage refrigeration unit: the conversion solution and the second-stage freezing crystallization mirabilite in the former step are used as stock solutions and enter a feeding tank 2, are fully dissolved by stirring and then enter a precooler 4 after passing through a feeding pump 3, and enter a first-stage freezing circulation pipeline after being subjected to heat exchange and cooling with second-stage freezing mother solution from a second-stage mother solution tank 23 in the precooler 4, and under the pushing of a first-stage freezing circulation pump 8, feed liquid enters a first-stage freezing heat exchanger 7 tube pass to exchange heat with a refrigerant in a shell pass, and enters a first-stage freezing crystallizer 9 for crystallization after being cooled; the refrigerant on the shell side of the primary refrigeration heat exchanger 7 circulates in a large amount under the action of a primary refrigerant circulating pump 6, so that the temperature is stable, and the low-temperature refrigerant is supplemented by a primary refrigerant pump 5 according to the heat absorbed in the heat exchange pipe to keep the temperature difference between the inside and the outside of the heat exchange pipe of the primary refrigeration heat exchanger 7; because the temperature of the primary freezing crystallizer 9 is reduced, mirabilite is continuously separated out, a large amount of crystal slurry containing mirabilite is pumped into a primary freezing thickener 11 through a primary freezing discharge pump 10 to further improve the concentration of the crystal slurry, and clear liquid returns to the primary freezing crystallizer 9 through an upper overflow port; the crystal slurry enters a first-stage centrifuge 12 for centrifugal separation, wherein solid mirabilite is discharged out of the system, and the mother liquor enters a first-stage mother liquor tank 13.
And (3) control points: the temperature in the primary freezing crystallizer 9 is controlled to be 5 ℃, the shell side temperature of the primary freezing heat exchanger 7 is controlled to be 0 ℃, the solid content of the slurry fed by the primary centrifuge 12 is 40%, the primary centrifuge 12 adopts a piston double-push centrifuge, and the water content of the separated crystals is less than 3%.
A secondary refrigeration unit: the primary refrigeration mother liquor enters a secondary refrigeration circulating pipeline through a primary mother liquor pump 14, under the pushing of a secondary refrigeration circulating pump, feed liquor enters a secondary refrigeration heat exchanger 17 tube pass to exchange heat with a refrigerant of a shell pass, and the feed liquor enters a secondary refrigeration crystallizer 19 for crystallization after being cooled; the refrigerant on the shell side of the secondary refrigeration heat exchanger 17 circulates in a large amount under the action of a secondary refrigerant circulating pump 16 to ensure stable temperature, and low-temperature refrigerant is supplemented by a secondary refrigerant pump 15 to keep the temperature difference between the inside and the outside of a heat exchange pipe of the secondary refrigeration heat exchanger 17 according to the heat absorbed in the heat exchange pipe; because the temperature of the secondary freezing crystallizer 19 is reduced, mirabilite is continuously separated out, a large amount of crystal slurry containing mirabilite is pumped into a secondary freezing thickener 21 through a secondary freezing discharge pump 20 to further improve the concentration of the crystal slurry, and clear liquid returns to the secondary freezing crystallizer 19 through an upper overflow port; the crystal slurry enters a secondary centrifuge 22 for centrifugal separation, wherein solid mirabilite enters a feeding tank 2; the mother liquor passes through a secondary mother liquor tank 23 and a secondary mother liquor pump 24, enters a precision filter 25 to separate mirabilite fine crystals, enters a precooler 4 to exchange heat with the raw materials, and is discharged out of the system.
And (3) control points: the temperature in the secondary freezing crystallizer 19 is controlled to be minus 7 ℃, the shell side temperature of the secondary freezing heat exchanger 17 is controlled to be minus 12 ℃, the solid content of the feed slurry of the secondary centrifuge 22 is 35 percent, the secondary centrifuge 22 adopts a spiral sedimentation filter centrifuge, and the separated mother liquor sodium sulfate is less than 1 percent.
The utility model discloses a theory of operation is: the utility model discloses a principle that reduces along with the reduction of temperature according to glauber's salt solubility, whole technology adopts the freezing method of two-stage, and wherein the freezing temperature of second grade is less than the one-level freezing, and the freezing difference in temperature of one-level is little, and solution volume is big, and the glauber's salt granule that consequently crystallizes out is big, and the water content is low to the lithium hydroxide that smugglies secretly is few, and the glauber's salt of crystallization can produce anhydrous sodium sulphate. The freezing mother liquor of one-level removes the further freezing mirabilite of second grade and separates out the glauber's salt, has taken out a large amount of water because of the glauber's salt is separated out, leads to lithium hydroxide content in the solution to improve, and the glauber's salt granule of crystallization is less relatively, and the moisture content is higher after centrifugal separation, and for reducing the lithium hydroxide loss, the glauber's salt that the second grade crystallization produced removes feed tank 2 and dissolves the recrystallization, and the second grade mother liquor has been taken off most glauber's salt, can regard as lithium hydroxide crystallization raw materials, just the utility model discloses in only have the output product of one-level, the second grade contains the crystal that the magazine is many then return to the stoste of foremost and dissolve the re-feeding.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A production process system for continuously removing Miscanthus sodium from a lithium hydroxide conversion solution is characterized by comprising a primary refrigeration unit and a secondary refrigeration unit; the primary refrigeration unit comprises a feeding tank, a feeding pump, a precooler, a primary refrigeration heat exchanger, a primary refrigeration crystallizer, a primary refrigeration discharge pump, a primary refrigeration thickener, a primary centrifuge, a primary mother liquor tank and a primary mother liquor pump which are connected in sequence; the secondary refrigeration unit comprises a secondary refrigeration heat exchanger, a secondary refrigeration crystallizer, a secondary refrigeration discharge pump, a secondary refrigeration thickener, a secondary centrifuge, a secondary mother liquor tank, a secondary mother liquor pump and a precision filter which are connected in sequence; the primary centrifuge is used for centrifugally separating the crystal slurry pumped into the primary centrifuge, the separated solid mirabilite is discharged out of the system as a product, and the primary mother liquor tank is used for collecting the mother liquor separated by the primary centrifuge; the primary mother liquor pump is used for driving primary freezing mother liquor in the primary mother liquor tank to enter a secondary freezing circulation pipeline, and the secondary freezing circulation pump is used for driving feed liquor entering the secondary freezing circulation pipeline to enter a tube side of the secondary freezing heat exchanger and exchange heat with a refrigerant of a shell side; the feeding tank is used for collecting the second-stage frozen crystal mirabilite separated by the second-stage centrifugal machine and the conversion liquid of the former process, and the second-stage frozen crystal mirabilite and the conversion liquid are used as stock solutions of the first-stage frozen crystal; the secondary mother liquor tank is used for collecting mother liquor separated by the secondary centrifuge, the secondary mother liquor pump is used for pumping the mother liquor collected in the secondary mother liquor tank into the precision filter, and the precooler is used for receiving mirabilite fine crystals separated by the precision filter and discharging the mirabilite fine crystals out of the system after heat exchange with the stock solution.
2. The system for continuously removing mirabilite from a lithium hydroxide conversion solution according to claim 1, wherein the primary freezing crystallizer is used for receiving feed liquid entering from a tube pass of the primary freezing heat exchanger and performing crystallization, the primary freezing circulating pump is used for pumping the feed liquid which is not crystallized in the primary freezing crystallizer into the tube pass of the primary freezing heat exchanger again to realize circulation of the feed liquid, and the tube pass of the primary freezing heat exchanger exchanges heat with refrigerant in a shell pass.
3. The system of claim 2, wherein the refrigerant in the shell side of the primary refrigeration heat exchanger is circulated in bulk by a primary refrigerant circulation pump, and is connected to the refrigerator by the primary refrigerant pump to supplement the low temperature refrigerant and maintain the temperature difference between the inside and the outside of the heat exchange tubes of the primary refrigeration heat exchanger.
4. The system for continuously removing mirabilite from lithium hydroxide conversion solution according to claim 1, wherein the circulation of feed liquid is realized between the secondary freezing heat exchanger and the secondary freezing crystallizer through a secondary freezing circulating pump, the feed liquid enters the tube side of the secondary freezing heat exchanger to exchange heat with the refrigerant on the shell side, and after cooling, the feed liquid enters the secondary freezing crystallizer to be crystallized.
5. The system of claim 4, wherein the refrigerant in the shell side of the secondary refrigerant heat exchanger is circulated in a large amount by a secondary refrigerant circulating pump, and the secondary refrigerant pump is connected to the refrigerator to supplement the low-temperature refrigerant and maintain the temperature difference between the inside and the outside of the heat exchange tubes of the secondary refrigerant heat exchanger.
CN202221406065.2U 2022-06-06 2022-06-06 Lithium hydroxide conversion solution continuous Miscanthus removal production process system Active CN217627643U (en)

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CN202221406065.2U CN217627643U (en) 2022-06-06 2022-06-06 Lithium hydroxide conversion solution continuous Miscanthus removal production process system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202221406065.2U CN217627643U (en) 2022-06-06 2022-06-06 Lithium hydroxide conversion solution continuous Miscanthus removal production process system

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CN217627643U true CN217627643U (en) 2022-10-21

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