CN215137034U - Glauber's salt serialization cooling crystallization equipment - Google Patents
Glauber's salt serialization cooling crystallization equipment Download PDFInfo
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- CN215137034U CN215137034U CN202120033747.2U CN202120033747U CN215137034U CN 215137034 U CN215137034 U CN 215137034U CN 202120033747 U CN202120033747 U CN 202120033747U CN 215137034 U CN215137034 U CN 215137034U
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Abstract
The application provides mirabilite continuous cooling crystallization equipment which comprises a primary cooling crystallizer and a secondary cooling crystallizer, wherein the primary cooling crystallizer comprises a first feeding hole, a first discharging hole, a first circulating liquid inlet and a first circulating liquid outlet, and the secondary cooling crystallizer comprises a second feeding hole, a second discharging hole, a second circulating liquid inlet and a second circulating liquid outlet; the stock solution is input into a first-stage cooling crystallizer through a first feed port, and a first discharge port is communicated with a second feed port through a pipeline; a first-stage cooling circulating pump and a first-stage cooling heat exchanger are connected between the first circulating liquid inlet and the first circulating liquid outlet, and a second-stage cooling circulating pump and a second-stage cooling heat exchanger are connected between the second circulating liquid inlet and the second circulating liquid outlet. The beneficial effect of this application is: the primary cooling crystallizer and the secondary cooling crystallizer are used for continuously cooling and crystallizing the stock solution, so that frequent start and stop of the equipment are avoided, the effective operation time of the equipment is prolonged, and the production efficiency is improved.
Description
Technical Field
The disclosure relates to the technical field of zero discharge of high-salinity wastewater and production and manufacturing of battery raw materials, in particular to mirabilite continuous cooling crystallization equipment.
Background
Natrii sulfas, also known as sodium sulfate decahydrate, has a chemical formula of Na2SO4.10H2O, crystal water content 55.9%, sodium sulfate content 44.1%.
With the increasing strictness of the national requirements on wastewater discharge, the zero discharge treatment of the wastewater of enterprises becomes a problem of great concern. As the industrial wastewater of chemical enterprises generally has the condition of high salt, the membrane method treatment is a main treatment mode, and the high-salt concentrated water generated by the membrane method treatment wastewater mainly contains sodium sulfate and other impurities. In order to improve the purity of the sodium sulfate and realize the change of waste into valuable, the sodium sulfate solution is cooled and crystallized to obtain mirabilite, and then the mirabilite is re-dissolved to obtain the high-purity sodium sulfate, which is an economic and effective method.
In addition, the lithium product has a very important position in modern industry, and has wide application in the fields of new energy and new materials, such as battery industry, ceramic industry, glass industry, aluminum industry, lubricants, medicines, refrigerants, nuclear industry, photoelectric industry and the like, the application range of the lithium product is continuously expanded, the demand is kept to be rapidly increased, and the industrial development prospect is very wide. At present, a sulfuric acid roasting-freezing method is a main method for producing lithium hydroxide in China, a denitration process of cooling and crystallizing mirabilite is a key link in the method, and the quality of mirabilite separated by the denitration process directly influences the quality of lithium and the yield of lithium.
In the traditional mirabilite crystallization method, a stirring kettle with a jacket or a coil pipe is usually used as a crystallizer, raw materials are added into the kettle at one time, then frozen brine is introduced into the jacket or the coil pipe of the crystallization kettle to exchange heat with a solution in the crystallization kettle, and after the temperature of materials in the kettle is reduced to a target temperature, a discharge valve is opened to discharge the materials to an intermittent centrifuge for solid-liquid separation. The intermittent mirabilite cooling and crystallizing process has the advantages of low heat exchange efficiency, long crystallizing time, frequent operation of workers, high labor intensity, high operation cost and incapability of continuous and normal production.
Disclosure of Invention
The utility model aims at above problem, provide a mirabilite serialization cooling crystallization equipment.
In a first aspect, the application provides mirabilite continuous cooling crystallization equipment, which comprises a primary cooling crystallizer and a secondary cooling crystallizer, wherein the primary cooling crystallizer comprises a first feeding hole, a first discharging hole, a first circulating liquid inlet and a first circulating liquid outlet, and the secondary cooling crystallizer comprises a second feeding hole, a second discharging hole, a second circulating liquid inlet and a second circulating liquid outlet;
the stock solution is input into the primary cooling crystallizer through a first feed port, and the first discharge port is communicated with a second feed port through a pipeline; be connected with one-level cooling circulating pump and one-level cooling heat exchanger between first circulation inlet and the first circulation liquid outlet, be connected with second grade cooling circulating pump and second grade cooling heat exchanger between second circulation inlet and the second circulation liquid outlet.
According to the technical scheme that this application embodiment provided, still include charge pump and mother liquor heat exchanger, in the input charge pump that the stoste passes through the charge pump, the output of charge pump passes through tube coupling to mother liquor heat exchanger's input, and mother liquor heat exchanger's output passes through tube coupling to the first feed inlet of one-level cooling crystallizer.
According to the technical scheme provided by the embodiment of the application, the device further comprises a primary discharging pump, a primary thickener, a primary centrifuge mother liquor tank and a primary centrifuge mother liquor pump; first discharge gate passes through the tube coupling to the input of one-level discharge pump, and the output of one-level discharge pump passes through the input of tube coupling to one-level thickener, and the output of one-level thickener passes through the tube coupling to one-level centrifuge's input, and the output of one-level centrifuge passes through the tube coupling to the input of one-level centrifugation mother liquor jar, and the output of one-level centrifugation mother liquor jar passes through the tube coupling to the second feed inlet.
According to the technical scheme provided by the embodiment of the application, the device further comprises a secondary discharging pump, a secondary thickener, a secondary centrifuge mother liquor tank and a secondary centrifuge mother liquor pump; the second discharge gate passes through the input of tube coupling to the second grade discharge pump, and the output of second grade discharge pump passes through the input of tube coupling to the second grade thickener, and the output of second grade thickener passes through the input of tube coupling to second grade centrifuge, and the output of second grade centrifuge passes through the input of tube coupling to second grade centrifugation mother liquor jar, and the output of second grade centrifugation mother liquor jar passes through the input of tube coupling to overflow mother liquor jar.
According to the technical scheme provided by the embodiment of the application, the output end of the overflow mother liquor tank is connected with the overflow mother liquor pump, and the output end of the overflow mother liquor pump is communicated with the mother liquor heat exchanger through a pipeline.
According to the technical scheme provided by the embodiment of the application, the primary cooling crystallizer and the secondary cooling crystallizer are set to be FC type crystallizers, DTB type crystallizers or OSLO type crystallizers.
According to the technical scheme provided by the embodiment of the application, the first-stage cooling heat exchanger and the second-stage cooling heat exchanger are arranged into vertical fixed tube-plate heat exchangers.
The invention has the beneficial effects that: the application provides a glauber's salt serialization cooling crystallization equipment carries out continuous cooling crystallization treatment to the stoste through one-level cooling crystallizer and second grade cooling crystallizer, has avoided equipment frequently to open and stop, has saved the human cost, has prolonged equipment effective operating duration, has improved production efficiency.
Drawings
FIG. 1 is a schematic structural diagram of a first embodiment of the present application;
the text labels in the figures are represented as: 1. a feed pump; 2. a mother liquor heat exchanger; 3. a primary cooling crystallizer; 4. a first-stage cooling circulating pump; 5. a first-stage cooling heat exchanger; 6. a first-level ice machine; 7. a first-stage frozen brine tank; 8. a first-stage chilled brine pump; 9. a primary discharge pump; 10. a first-stage thickener; 11. a primary centrifuge; 12. a first-stage centrifugal mother liquor tank; 13. a primary centrifugal mother liquor pump; 14. a secondary cooling crystallizer; 15. a second-stage cooling circulating pump; 16. a secondary cooling heat exchanger; 17. a secondary ice maker; 18. a secondary frozen brine tank; 19. a secondary chilled brine pump; 20. a secondary discharge pump; 21. a secondary thickener; 22. a secondary centrifuge; 23. a secondary centrifugal mother liquor tank; 24. a secondary centrifugal mother liquor pump; 25. an overflow mother liquor tank; 26. and (4) an overflow mother liquor pump.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following detailed description of the present invention is provided in conjunction with the accompanying drawings, and the description of the present section is only exemplary and explanatory, and should not be construed as limiting the scope of the present invention in any way.
Fig. 1 is a schematic diagram of a first embodiment of the present application, which includes a primary cooling crystallizer 3 and a secondary cooling crystallizer 14, where the primary cooling crystallizer 3 includes a first feeding port, a first discharging port, a first circulating liquid inlet, and a first circulating liquid outlet, and the secondary cooling crystallizer 14 includes a second feeding port, a second discharging port, a second circulating liquid inlet, and a second circulating liquid outlet;
the stock solution is input into the primary cooling crystallizer 3 through a first feed port, and the first discharge port is communicated with a second feed port through a pipeline; be connected with one-level cooling circulating pump 4 and one-level cooling heat exchanger 5 between first circulation inlet and the first circulation liquid outlet, be connected with second grade cooling circulating pump 15 and second grade cooling heat exchanger 16 between second circulation inlet and the second circulation liquid outlet.
In a preferred embodiment, the primary cooling crystallizer 3 and the secondary cooling crystallizer 14 are FC type crystallizers, DTB type crystallizers or OSLO type crystallizers. The FC type crystallizer, the DTB type crystallizer or the OSLO type crystallizer are beneficial to crystal nucleation and growth, and crystals with larger grain diameter can be obtained.
In a preferred embodiment, the primary cooling heat exchanger 5 and the secondary cooling heat exchanger 16 are vertical fixed-tube plate heat exchangers. The fixed tube-sheet heat exchanger has the advantages of simple structure, low manufacturing cost, convenient tube side cleaning, wide specification range and 20-30% larger heat transfer area than the floating head heat exchanger.
In this embodiment, the stock solution enters into one-level cooling crystallizer 3 from first feed inlet, and the stock solution flows out through first circulation liquid outlet and squeezes into one-level cooling heat exchanger 5 in through one-level cooling circulating pump 4, and the velocity of flow in the pipeline that one-level cooling crystallizer 3 and one-level cooling heat exchanger 5 are connected reaches 2.1-2.2m/s, can effectively avoid heat transfer pipeline inner wall scale deposit. The stock solution is circularly input into the primary cooling crystallizer 3 again through the first circulating liquid inlet after being cooled by the primary cooling heat exchanger 5. Feed liquid output by a first discharge port of the primary cooling crystallizer 3 enters the secondary cooling crystallizer 14 through a second feed port, the feed liquid flows out through a second circulating liquid outlet and is pumped into the secondary cooling heat exchanger 16 through the secondary cooling circulating pump 15, the flow velocity in a pipeline connecting the secondary cooling crystallizer 14 and the secondary cooling heat exchanger 16 reaches 2.1-2.2m/s, and scaling of the inner wall of the heat exchange pipeline can be effectively avoided. The feed liquid is circularly input into the secondary cooling crystallizer 14 again through the second circulating liquid inlet after being cooled by the secondary cooling heat exchanger 16.
In the embodiment, a cold source of the primary cooling heat exchanger 5 is frozen brine stored in a primary frozen brine tank 7, the frozen brine is conveyed to a primary ice maker 6 through a primary frozen brine pump 8, the primary cooling heat exchanger 5 exchanges heat after the primary ice maker 6 works, and the primary cooling crystallization temperature is guaranteed to be 10 ℃; the cold source of the secondary cooling heat exchanger 16 is frozen brine stored in a secondary frozen brine tank 18, the frozen brine is conveyed to a secondary ice maker 17 through a secondary frozen brine pump 19, the secondary cooling heat exchanger 16 exchanges heat after the secondary ice maker 17 works, and the secondary cooling crystallization temperature is guaranteed to be-10 ℃.
In a preferred embodiment, the equipment further comprises a feed pump 1 and a mother liquor heat exchanger 2, the stock solution is input into the feed pump 1 through the input end of the feed pump 1, the output end of the feed pump 1 is connected to the input end of the mother liquor heat exchanger 2 through a pipeline, and the output end of the mother liquor heat exchanger 2 is connected to the first feed inlet of the primary cooling crystallizer 3 through a pipeline.
In a preferred embodiment, the equipment further comprises a primary discharge pump 9, a primary thickener 10, a primary centrifuge 11, a primary centrifuge mother liquor tank 12 and a primary centrifuge mother liquor pump 13; first discharge gate passes through the tube coupling to the input of one-level discharge pump 9, and the output of one-level discharge pump 9 passes through the tube coupling to the input of one-level thickener 10, and the output of one-level thickener 10 passes through the tube coupling to the input of one-level centrifuge 11, and the output of one-level centrifuge 11 passes through the tube coupling to the input of one-level centrifugation mother liquor jar 12, and the output of one-level centrifugation mother liquor jar 12 passes through the tube coupling to the input of one-level centrifugation mother liquor jar 13, and the output of one-level centrifugation mother liquor jar 13 passes through the tube coupling to the second feed inlet.
In a preferred embodiment, the equipment further comprises a secondary discharge pump 20, a secondary thickener 21, a secondary centrifuge 22, a secondary centrifuge mother liquor tank 23 and a secondary centrifuge mother liquor pump 24; the second discharge gate passes through the input of tube coupling to second grade discharge pump 20, the output of second grade discharge pump 20 passes through the input of tube coupling to second grade thickener 21, the output of second grade thickener 21 passes through the input of tube coupling to second grade centrifuge 22, the output of second grade centrifuge 22 passes through the input of tube coupling to second grade centrifugation mother liquor jar 23, the output of second grade centrifugation mother liquor jar 23 passes through the input of tube coupling to second grade centrifugation mother liquor jar 24, the output of second grade centrifugation mother liquor jar 24 passes through the input of tube coupling to overflow mother liquor jar 25.
In the above preferred embodiment, preferably, the output end of the overflow mother liquor tank 25 is connected to an overflow mother liquor pump 26, and the output end of the overflow mother liquor pump 26 is communicated with the mother liquor heat exchanger 2 through a pipeline.
The process for carrying out continuous cooling crystallization of mirabilite by using the crystallization equipment comprises the following steps:
s1, inputting the sodium sulfate stock solution into a mother solution heat exchanger 2 through a feed pump 1, wherein cold sources of the heat exchanger are overflow mother solution and centrifugal mother solution generated by system evaporation, and the mother solution heat exchanger 2 is used for cooling the stock solution to 20-25 ℃.
S2, conveying the sodium sulfate stock solution subjected to mother liquor heat exchange into a primary cooling crystallizer 3, pumping the stock solution into a primary cooling heat exchanger 5 through a primary cooling circulating pump 4, wherein the flow velocity in a heat exchange tube reaches 2.1-2.2m/S, and scaling on the inner wall of the heat exchange tube can be effectively avoided; exchanging heat with chilled water in a primary cooling crystallizer 3 to cool to 10 ℃, and separating out Na2SO4.10H2O; na is precipitated2SO4.10H2The O crystal slurry enters a first-stage thickener 10 for thickening through a first-stage discharge pump 9, enters a first-stage centrifuge 11 for dehydration after the solid-liquid ratio of the first-stage thickener 10 reaches 40% -50%, and Na is obtained after dehydration2SO4.10H2O accounts for about 60% of the total crystal amount.
S3, allowing the centrifugal mother liquor generated by the primary centrifuge 11 to enter a primary centrifugal mother liquor tank 12, conveying the centrifugal mother liquor to a secondary cooling crystallizer 14 by a primary centrifugal mother liquor pump 13, pumping the feed liquor into a secondary cooling heat exchanger 16 through a secondary cooling circulating pump 15, performing heat exchange between the feed liquor and chilled water in the secondary cooling crystallizer 14, cooling to-10 ℃, and separating out Na2SO4.10H2O; na is precipitated2SO4.10H2The O crystal slurry enters a secondary thickener 21 for thickening through a secondary discharge pump 20, enters a secondary centrifuge 22 for dehydration when the solid-liquid ratio of the secondary thickener 21 reaches 40-50 percent, and Na is added after the dehydration2SO4.10H2O accounts for about 40% of the total crystal amount.
S4, centrifugal mother liquor generated by the secondary centrifuge 22 enters a secondary centrifugal mother liquor tank 23, is conveyed to an overflow mother liquor tank 25 by a secondary centrifugal mother liquor pump 24, and is conveyed to a mother liquor heat exchanger 2 by an overflow mother liquor pump to exchange heat with the raw liquor, so that energy can be saved to a great extent.
The principles and embodiments of the present application are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present application. The foregoing is only a preferred embodiment of the present application, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present application, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments, or may be learned by practice of the invention.
Claims (7)
1. A mirabilite continuous cooling crystallization device is characterized by comprising a primary cooling crystallizer and a secondary cooling crystallizer, wherein the primary cooling crystallizer comprises a first feeding hole, a first discharging hole, a first circulating liquid inlet and a first circulating liquid outlet, and the secondary cooling crystallizer comprises a second feeding hole, a second discharging hole, a second circulating liquid inlet and a second circulating liquid outlet;
the stock solution is input into the primary cooling crystallizer through a first feed port, and the first discharge port is communicated with a second feed port through a pipeline; be connected with one-level cooling circulating pump and one-level cooling heat exchanger between first circulation inlet and the first circulation liquid outlet, be connected with second grade cooling circulating pump and second grade cooling heat exchanger between second circulation inlet and the second circulation liquid outlet.
2. The mirabilite continuous cooling crystallization device according to claim 1, further comprising a feed pump and a mother liquor heat exchanger, wherein the stock solution is input into the feed pump through an input end of the feed pump, an output end of the feed pump is connected to an input end of the mother liquor heat exchanger through a pipeline, and an output end of the mother liquor heat exchanger is connected to the first feed inlet of the primary cooling crystallizer through a pipeline.
3. The mirabilite continuous cooling crystallization device according to claim 2, further comprising a primary discharge pump, a primary thickener, a primary centrifuge mother liquor tank and a primary centrifuge mother liquor pump; first discharge gate passes through the tube coupling to the input of one-level discharge pump, and the output of one-level discharge pump passes through the input of tube coupling to one-level thickener, and the output of one-level thickener passes through the tube coupling to one-level centrifuge's input, and the output of one-level centrifuge passes through the tube coupling to the input of one-level centrifugation mother liquor jar, and the output of one-level centrifugation mother liquor jar passes through the tube coupling to the second feed inlet.
4. The mirabilite continuous cooling crystallization device according to claim 3, further comprising a secondary discharge pump, a secondary thickener, a secondary centrifuge mother liquor tank and a secondary centrifuge mother liquor pump; the second discharge gate passes through the input of tube coupling to the second grade discharge pump, and the output of second grade discharge pump passes through the input of tube coupling to the second grade thickener, and the output of second grade thickener passes through the input of tube coupling to second grade centrifuge, and the output of second grade centrifuge passes through the input of tube coupling to second grade centrifugation mother liquor jar, and the output of second grade centrifugation mother liquor jar passes through the input of tube coupling to overflow mother liquor jar.
5. The mirabilite continuous cooling crystallization device according to claim 4, characterized in that the output end of the overflow mother liquor tank is connected with an overflow mother liquor pump, and the output end of the overflow mother liquor pump is communicated with the mother liquor heat exchanger through a pipeline.
6. The mirabilite continuous cooling crystallization device according to any one of claims 1 to 5, wherein the primary cooling crystallizer and the secondary cooling crystallizer are configured as FC type crystallizer, DTB type crystallizer or OSLO type crystallizer.
7. The mirabilite continuous cooling crystallization device according to any one of claims 1 to 5, wherein the primary cooling heat exchanger and the secondary cooling heat exchanger are vertical fixed tube-plate heat exchangers.
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| CN202120033747.2U CN215137034U (en) | 2021-01-07 | 2021-01-07 | Glauber's salt serialization cooling crystallization equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115448375A (en) * | 2022-09-13 | 2022-12-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for continuously crystallizing ferrous sulfate in titanium white and titanium liquid by sulfuric acid method |
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2021
- 2021-01-07 CN CN202120033747.2U patent/CN215137034U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115448375A (en) * | 2022-09-13 | 2022-12-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for continuously crystallizing ferrous sulfate in titanium white and titanium liquid by sulfuric acid method |
| CN115448375B (en) * | 2022-09-13 | 2023-11-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for continuously crystallizing ferrous sulfate in sulfuric acid process titanium dioxide titanium liquid |
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