CN114917600A - Evaporative crystallization process and device for producing borax from salt lake lithium extraction discharge liquid - Google Patents
Evaporative crystallization process and device for producing borax from salt lake lithium extraction discharge liquid Download PDFInfo
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- CN114917600A CN114917600A CN202210620993.7A CN202210620993A CN114917600A CN 114917600 A CN114917600 A CN 114917600A CN 202210620993 A CN202210620993 A CN 202210620993A CN 114917600 A CN114917600 A CN 114917600A
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- 239000007788 liquid Substances 0.000 title claims abstract description 62
- 229910021538 borax Inorganic materials 0.000 title claims abstract description 55
- 235000010339 sodium tetraborate Nutrition 0.000 title claims abstract description 55
- 239000004328 sodium tetraborate Substances 0.000 title claims abstract description 55
- 238000002425 crystallisation Methods 0.000 title claims abstract description 40
- 230000008025 crystallization Effects 0.000 title claims abstract description 40
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 33
- 238000000605 extraction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000008569 process Effects 0.000 title claims abstract description 26
- 239000011552 falling film Substances 0.000 claims abstract description 152
- 238000001704 evaporation Methods 0.000 claims abstract description 37
- 230000008020 evaporation Effects 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 38
- 239000013078 crystal Substances 0.000 claims description 34
- 239000012452 mother liquor Substances 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 17
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 15
- 229910052796 boron Inorganic materials 0.000 claims description 15
- 239000002351 wastewater Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
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- 238000001816 cooling Methods 0.000 claims description 8
- 230000008719 thickening Effects 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
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- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 description 3
- RSCACTKJFSTWPV-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 RSCACTKJFSTWPV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 2
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- 239000012141 concentrate Substances 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical group [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- B01D1/0011—Heating features
- B01D1/0041—Use of fluids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0094—Evaporating with forced circulation
-
- 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
- B01D1/28—Evaporating with vapour compression
-
- 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
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/121—Borates of alkali metal
- C01B35/122—Sodium tetraborates; Hydrates thereof, e.g. borax
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/121—Borates of alkali metal
- C01B35/122—Sodium tetraborates; Hydrates thereof, e.g. borax
- C01B35/124—Preparation by working up natural brines, e.g. seawater
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/08—Thin film evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/108—Boron compounds
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Hydrology & Water Resources (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses an evaporative crystallization process and a device for producing borax from lithium extraction discharge liquid of a salt lake. The two-stage MVR combined evaporator can adopt a combination of a one-stage single-effect falling-film evaporator and a one-stage forced circulation evaporator, and can also adopt a combination of a one-stage double-effect falling-film evaporator and a one-stage forced circulation evaporator. The process of the invention provides a two-stage MVR combined evaporator evaporation concentration mode to produce borax from the salt lake lithium extraction discharge liquid, thereby improving the economic benefit and the environmental benefit of enterprises.
Description
Technical Field
The invention relates to the technical field of resources and environment, in particular to an evaporative crystallization process and device for producing borax from a lithium extraction effluent of a salt lake.
Background
The chemical composition of borax is sodium tetraborate, mainly present in mineral deposits. Borax is commonly used in glass production, and can enhance the transmittance of glass to ultraviolet rays and improve the transparency and heat resistance of glass. In enamel products, borax can make enamel not easy to fall off and make the enamel glossy. Borax has antiseptic effect, and can be used for relieving inflammation and sterilizing in medicine field. Borax is also widely used in the fields of chemical industry, metallurgy, military industry, machinery and the like. It follows that boron-containing products occupy a very important position in various fields. If the boron-containing wastewater discharged in the production of extracting lithium from the salt lake can be treated to obtain high-purity borax which is recycled, the economic benefit of enterprises and the utilization rate of salt lake resources can be greatly improved.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an evaporative crystallization process and a device for producing borax from a lithium extraction discharge liquid in a salt lake.
The technical scheme adopted by the invention is as follows:
an evaporative crystallization process and a device for producing borax from a salt lake lithium extraction discharge liquid comprise: the concentration section adopts a two-stage MVR combined evaporator to carry out evaporation concentration on the boron-containing wastewater; the crystallization section adopts a cooling crystallization mode to produce borax crystals; wherein:
the two-stage MVR combined evaporator of the concentration section adopts a combination of a first-stage falling film evaporator and a second-stage forced circulation evaporator; the first-stage falling-film evaporator at least comprises a single-effect falling-film evaporator; or the first-stage falling-film evaporator adopts a mode of connecting two-effect falling-film evaporators in series;
when the two-stage MVR combined evaporator adopts the combination of a one-stage single-effect falling-film evaporator and a two-stage forced circulation evaporator, the concentration mode comprises the following steps:
the preheated boron-containing wastewater enters a first-stage single-effect falling-film evaporator for heating and evaporation, and secondary steam generated by the evaporator enters an MVR steam compressor;
the feed liquid concentrated by the first-stage single-effect falling-film evaporator enters a second-stage forced circulation evaporator for evaporation and concentration, and secondary steam generated by the evaporator enters the MVR steam compressor;
the secondary steam compressed by the MVR steam compressor enters the primary single-effect falling-film evaporator and the secondary forced circulation evaporator to be used as heating steam;
the discharge of the second-stage forced circulation evaporator enters a crystallizer for cooling crystallization;
the crystal slurry generated by the crystallizer enters a centrifugal machine for solid-liquid separation, and a borax product is separated;
when the two-stage MVR combined evaporator is a combination of a first-stage double-effect falling film evaporator and a second-stage forced circulation evaporator, the concentration mode comprises the following steps:
the preheated boron-containing wastewater enters a first-stage one-effect falling-film evaporator for heating and evaporation, the generated secondary steam enters a steam inlet of a first-stage two-effect falling-film evaporator to be used as a heat source, and the feed liquid concentrated by the first-stage one-effect falling-film evaporator enters the first-stage two-effect falling-film evaporator for heating and evaporation;
the secondary steam generated by the first-stage two-effect falling-film evaporator enters an MVR steam compressor;
the feed liquid concentrated by the first-stage two-effect falling-film evaporator enters a second-stage forced circulation evaporator for evaporation and concentration, and secondary steam generated by the evaporator enters the MVR steam compressor;
the secondary steam compressed by the MVR steam compressor enters the primary one-effect falling-film evaporator and the secondary forced circulation evaporator to be used as heating steam;
the discharge of the secondary forced circulation evaporator enters a crystallizer for cooling crystallization;
and (4) feeding crystal slurry generated by crystallization of the crystallizer into a centrifugal machine for solid-liquid separation to separate a borax product.
Preferably, the boron-containing wastewater is preheated by a primary preheater and a secondary preheater which are sequentially connected, and the feed liquid preheated by the secondary preheater enters the primary falling-film evaporator.
Preferably, the non-condensable gas generated by the first-stage falling-film evaporator and the second-stage forced circulation evaporator is recycled to enter the second-stage preheater for preheating.
Preferably, the condensed water generated by the first-stage falling-film evaporator, the second-stage forced circulation evaporator and the second-stage preheater is recycled to enter a condensed water tank and then enters the first-stage preheater for preheating.
Preferably, the non-condensable gas generated by the secondary preheater enters a condenser, and condensed condensate water enters the primary preheater for preheating.
Preferably, the crystallizer adopts a jacket crystal slurry tank, the crystal slurry tank is cooled by circulating cooling water to separate out crystals, the purposes of thickening and crystal growing are achieved, and then the crystals enter a centrifugal machine to carry out solid-liquid separation.
Preferably, the mother liquor separated by the centrifuge is partially returned to the secondary forced circulation evaporator and partially discharged.
An MVR system for producing borax from a salt lake lithium extraction discharge solution comprises an MVR evaporation concentration system consisting of a first-stage single-effect falling film evaporator or a first-stage double-effect falling film and a second-stage forced circulation evaporator, wherein:
the MVR concentration system composed of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator comprises:
a first-stage single-effect falling-film evaporator;
the discharge port of the primary single-effect falling-film evaporator is connected with the feed port of the secondary forced circulation evaporator;
a vapor inlet of the MVR vapor compressor is connected with vapor outlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator; the steam outlet of the MVR steam compressor is connected with the steam inlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator;
the feed inlet of the crystallizer is connected with the discharge outlet of the secondary forced circulation evaporator;
the feed inlet of the centrifuge is connected with the discharge outlet of the crystallizer, the solid discharge outlet of the centrifuge discharges borax, and the liquid discharge outlet of the centrifuge is connected with the mother liquor tank;
the MVR evaporation concentration system composed of the first-stage double-effect falling-film evaporator and the second-stage forced circulation evaporator comprises:
a first-stage double-effect falling-film evaporator; the primary double-effect falling-film evaporator comprises a primary one-effect falling-film evaporator and a primary two-effect falling-film evaporator, a steam outlet of the primary one-effect falling-film evaporator is connected with a steam inlet of the primary two-effect falling-film evaporator, and a discharge outlet of the primary one-effect falling-film evaporator is connected with a feed inlet of the primary two-effect evaporator;
the discharge hole of the first-stage two-effect falling-film evaporator is connected with the feed hole of the second-stage forced circulation evaporator;
a vapor inlet of the MVR vapor compressor is connected with a vapor outlet of the first-stage two-effect falling-film evaporator and a vapor outlet of the second-stage forced circulation evaporator, and a vapor outlet of the MVR vapor compressor is connected with a vapor inlet of the first-stage one-effect falling-film evaporator and a vapor inlet of the second-stage forced circulation evaporator;
the discharge port of the secondary forced circulation evaporator is connected with the feed port of the crystallizer;
the centrifuge, centrifuge's pan feeding mouth with the discharge gate of crystallizer is connected, centrifuge's solid discharge gate discharges, centrifuge's liquid discharge gate is connected with the mother liquor jar.
Preferably, an outlet of the mother liquor tank is respectively connected with the secondary forced circulation evaporator and the discharge device. Preferably, the system further comprises a first-stage preheater and a second-stage preheater which are connected, and the second-stage preheater is connected with a feed inlet of the first-stage falling-film evaporator.
Preferably, the non-condensable gas outlets of the first-stage falling-film evaporator and the second-stage forced circulation evaporator are connected with the inlet of the second-stage preheater.
Preferably, the non-condensable gas outlet of the secondary preheater is connected with the inlet of a condenser, and the outlet of the condenser is connected with the inlet of the primary preheater.
Preferably, the condensed water outlets of the first-stage falling-film evaporator and the second-stage forced circulation evaporator are connected with the inlet of a condensed water tank, and the outlet of the condensed water tank is connected with the inlet of the first-stage preheater.
The invention provides a two-stage MVR combined evaporator, which comprises an MVR evaporation concentration system and a cooling crystallization system, wherein the MVR evaporation concentration system consists of a first-stage falling-film evaporator and a second-stage forced circulation evaporator, borax is produced from a lithium extraction discharge liquid in a salt lake, and the economic benefit and the environmental benefit of an enterprise are improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a working principle diagram of an evaporative crystallization process and an apparatus for producing borax from a lithium extraction effluent of a salt lake according to an embodiment of the present invention (MVR system combining a first-stage single-effect falling film evaporator and a second-stage forced circulation evaporator).
Fig. 2 is a schematic diagram of an evaporative crystallization process and an apparatus for producing borax from a lithium extraction effluent of a salt lake according to another embodiment of the present invention (MVR system combining a primary double-effect falling-film evaporator and a secondary forced circulation evaporator).
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
Referring to fig. 1, the embodiment of the invention provides an evaporative crystallization process and a device for producing borax from a lithium extraction discharge liquid in a salt lake.
Specifically, as shown in fig. 1, the technology is matched with an evaporative crystallization device for producing borax from the lithium extraction effluent of a salt lake to realize the functions. The evaporative crystallization process and the device for producing borax from the salt lake lithium extraction discharge liquid comprise a first-stage single-effect falling-film evaporator, a second-stage forced circulation evaporator and an MVR steam compressor, wherein a discharge port of the first-stage single-effect falling-film evaporator is communicated with a feed port of the second-stage forced circulation evaporator. The vapor inlet of the MVR vapor compressor is respectively connected with the vapor outlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator, and the vapor outlet of the MVR vapor compressor is respectively connected with the vapor inlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator. Specifically, secondary steam generated by evaporation in the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator is separated by a gas-liquid separator and then enters an MVR steam compressor, the low-pressure secondary steam is subjected to pressure boosting and temperature rising in the MVR steam compressor, and the compressed secondary steam is conveyed into the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator through a steam outlet of the MVR steam compressor to serve as heating steam of the two-stage evaporator and participate in evaporation concentration of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator. Therefore, the process can compress and recycle all secondary steam by adopting the MVR technology, thereby greatly saving the steam energy and having large evaporation capacity of the system; and the investment cost of the equipment is low, the occupied area is small, and the maintenance and operation personnel are few.
Further, the feed inlet of the first-stage single-effect falling-film evaporator is communicated with the discharge outlet of the second-stage preheater, the feed inlet of the second-stage preheater is communicated with the discharge outlet of the first-stage preheater, and the feed inlet of the first-stage preheater is communicated with the discharge outlet of the feed tank. The material (boron-containing wastewater) sent by the feeding tank enters a first-stage preheater through an electromagnetic flow meter and an automatic regulating valve by a feeding pump, is preheated to a certain temperature and then enters a discharging bin of a first-stage single-effect falling-film evaporator.
Further, the discharge hole of the first-stage single-effect falling-film evaporator is communicated with the feed hole of the second-stage forced circulation evaporator, the discharge hole of the second-stage forced circulation evaporator is communicated with the crystallizer, and the discharge hole of the crystallizer is communicated with the feed hole of the centrifugal machine. After the material is evaporated and concentrated by the first-stage single-effect falling-film evaporator, the material reaches the designed concentration and is conveyed to the second-stage forced circulation evaporator by the material passing pump. The material passing regulating valve and the forced circulation evaporator liquid level sensor are interlocked and automatically controlled. After the concentration of the two-stage evaporator reaches the designed concentration, the mixture is conveyed to a crystallizer by a discharge pump, the crystallizer adopts a jacket crystal slurry tank, the jacket of the crystal slurry tank is filled with circulating cooling water for cooling, crystals are separated out, the purposes of thickening and crystal growing are achieved, and then the crystals enter a centrifugal machine for solid-liquid separation. Discharging borax from a solid discharge port of the centrifugal machine; the liquid discharge port of the centrifuge is communicated with the inlet of the mother liquor tank, and the outlet of the mother liquor tank is respectively communicated with the feed port of the secondary forced circulation evaporator and the discharge device. Most of the mother liquor separated by the centrifuge returns to the evaporator system for further evaporation and concentration, and a small part of the mother liquor is discharged out of the system for treatment through an external discharge device, wherein the external discharge device can be a conveying pipeline or a storage tank. Wherein, when the temperature of the crystallizer is controlled to be above 60 ℃, borax pentahydrate can be crystallized; when the temperature of the crystallizer is controlled below 60 ℃, borax decahydrate can be crystallized.
Further, condensed water outlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator are communicated with an inlet of a condensed water tank, an outlet of the condensed water tank is communicated with a heat source inlet of the first-stage preheater, condensed water generated by the second-stage evaporator can be used as a heat source of the first-stage preheater after being mixed in a condensed water storage tank, and preferably, noncondensable gas outlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator are communicated with an inlet of the second-stage preheater to be used as a heat source of the second-stage preheating, a noncondensable gas outlet of the second-stage preheater is communicated with an inlet of a condenser, and an outlet of the condenser is communicated with an inlet of the first-stage preheater to be used as a heat source of the first-stage preheating. The process has low operation cost, less condensed water consumption, high energy utilization rate and high economic benefit.
The specific steps of the evaporative crystallization process and the device for producing borax from the lithium extraction effluent of the salt lake provided by the embodiment of the present invention are described as follows in combination with the evaporative crystallization process and the device for producing borax from the lithium extraction effluent of the salt lake provided by the embodiment 1:
the first step is as follows: the preheated boron-containing wastewater enters a primary single-effect falling-film evaporator, raw steam (or secondary steam after mechanical compression) is used as a heat source, the heated solution reaches a certain temperature under a specific pressure, water is evaporated to generate secondary steam, and primary evaporation concentration of materials is carried out to reach a designed concentration;
the second step: the material evaporated and concentrated by the first-stage single-effect falling-film evaporator is conveyed to a second-stage forced circulation evaporator by a material passing pump, secondary steam generated by the second-stage forced circulation evaporator and secondary steam generated by the first-stage single-effect falling-film evaporator enter an MVR steam compressor together for compression and temperature rise, and then return to the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator to be used as heat sources again; a material passing regulating valve is arranged behind a material discharging and passing pump of the primary single-effect falling-film evaporator and is in linkage automatic control with a liquid level sensor of the secondary forced circulation evaporator, when the liquid level of the secondary forced circulation evaporator reaches a set liquid level, the material passing regulating valve is opened, and the material passing pump starts to convey materials into the secondary forced circulation evaporator;
the third step: the material after the second-stage forced circulation evaporator is evaporated and concentrated to reach the designed concentration enters a crystallizer, the crystallizer adopts a jacket crystal slurry tank, and a cooling water is introduced into a jacket of the crystal slurry tank for cooling, so that crystals are separated out, and the purposes of thickening and growing the crystals are achieved.
The fourth step: conveying the crystal slurry from the crystallizer to a centrifugal machine for solid-liquid separation, wherein the separated solid is borax; the separated liquid enters a mother liquor tank, most of the mother liquor returns to the secondary forced circulation evaporator to continue evaporation and concentration, and a small part of the mother liquor is discharged for treatment.
Further, in the first step, the boron-containing wastewater is preheated in two stages by adopting a first-stage preheater and a second-stage preheater which are sequentially connected, and the preheating temperature is gradually increased without crystallization. The condensate water generated by the primary single-effect falling-film evaporator and the secondary forced circulation evaporator is mixed in a condensate water storage tank and then enters the primary preheater, and the condensate water is used as a heat source of the primary preheater to recycle the waste heat and then is sent out of the system. The non-condensable gas generated by the primary single-effect falling-film evaporator and the secondary forced circulation evaporator enters the secondary preheater and is used as a heat source of the secondary preheater to recycle waste heat, condensed water discharged by the secondary preheater enters the condensed water tank, is mixed with the condensed water discharged by the primary single-effect falling-film evaporator and the secondary forced circulation evaporator in the condensed water tank, and then enters the primary preheater, so that the condensed water generated in the system and the waste heat of the non-condensable gas are fully recycled.
Example 2:
when a large amount of moisture needs to be evaporated, in order to greatly reduce energy consumption and improve the production efficiency of borax, an MVR evaporation concentration mode combining a first-stage double-effect falling-film evaporator and a second-stage forced circulation evaporator can also be adopted. Referring to fig. 2, the evaporative crystallization process and the device for producing borax from the lithium extraction discharge liquid of the salt lake comprise a first-stage one-effect falling-film evaporator, a first-stage two-effect falling-film evaporator, a second-stage forced circulation evaporator and an MVR steam compressor.
The steam outlet of this one-level one-effect falling-film evaporator is connected with the steam inlet of one-level two-effect falling-film evaporator, the discharge gate of one-level one-effect falling-film evaporator is connected with the pan feeding mouth of one-level two-effect falling-film evaporator, the steam outlet of this one-level two-effect falling-film evaporator is connected with MVR vapor compressor's steam inlet, this MVR vapor compressor's steam outlet is connected with the steam inlet of one-level one-effect falling-film evaporator and the steam inlet of second grade forced circulation evaporimeter respectively, the steam outlet of second grade forced circulation evaporimeter also is connected with this MVR vapor compressor steam inlet.
Specifically, secondary steam generated by evaporation in the first-stage one-effect falling-film evaporator is used as a heat source and supplied to the first-stage two-effect falling-film evaporator to continuously evaporate and concentrate the material liquid, the secondary steam generated by the first-stage two-effect falling-film evaporator enters the MVR steam compressor, low-pressure secondary steam is subjected to pressure boosting and temperature rising in the MVR steam compressor, and the compressed secondary steam is conveyed to the first-stage one-effect falling-film evaporator and the second-stage forced circulation evaporator through a steam outlet of the MVR steam compressor and is used as heating steam for two-stage evaporation to participate in the evaporation and concentration of the first-stage falling-film evaporator and the second-stage forced circulation evaporator. Meanwhile, secondary steam generated by the second-stage forced circulation evaporator also enters the MVR steam compressor, and returns to the first-stage first-effect falling-film evaporator and the second-stage forced circulation evaporator after being compressed. Therefore, the process can compress and recycle all secondary steam by adopting the MVR technology, thereby greatly saving the steam energy and having large evaporation capacity of the system; the first-stage falling-film evaporator adopts the two-effect series falling-film evaporators, so that the amount of secondary steam entering the compressor is reduced, the investment cost of the compressor can be reduced, the operation energy consumption is greatly reduced, the occupied area of equipment is small, and the number of maintenance and operation personnel is small.
Further, a discharge port of the second-stage forced circulation evaporator is connected with the crystallizer, a discharge port of the crystallizer is connected with a feed port of the centrifuge, a solid discharge port of the centrifuge discharges borax, and a liquid discharge port of the centrifuge is communicated with the mother liquor tank. The discharge hole of the mother liquor tank is respectively connected with a mother liquor inlet of the secondary forced circulation evaporator and an external discharge device. Wherein, when the temperature of the crystallizer is controlled to be above 60 ℃, borax pentahydrate can be crystallized; when the temperature of the crystallizer is controlled below 60 ℃, borax decahydrate can be crystallized.
Furthermore, a feed inlet of the first-stage first-effect falling-film evaporator is communicated with a discharge outlet of the second-stage preheater, a feed inlet of the second-stage preheater is communicated with a discharge outlet of the first-stage preheater, and a feed inlet of the first-stage preheater is communicated with a discharge outlet of the feed tank. The material (wastewater containing borax) sent from the feeding tank enters a first-stage preheater through an electromagnetic flowmeter and an automatic regulating valve by a feeding pump, is preheated to a certain temperature and then enters a discharging bin of a first-stage one-effect falling film evaporator.
Further, a discharge port of the first-stage one-effect falling-film evaporator is communicated with a feed port of the first-stage two-effect falling-film evaporator, a discharge port of the first-stage two-effect falling-film evaporator is communicated with a feed port of the second-stage forced circulation evaporator, a discharge port of the second-stage forced circulation evaporator is communicated with the crystallizer, and a discharge port of the crystallizer is communicated with a feed port of the centrifugal machine. After the material is evaporated and concentrated by the primary one-effect falling-film evaporator, the material is conveyed to the primary two-effect falling-film evaporator after reaching the designed concentration and adjusted by the material passing adjusting valve, and the material passing adjusting valve is automatically controlled by a liquid level sensor of the primary two-effect falling-film evaporator in a linkage manner; and the material reaching the designed concentration in the first-stage two-effect falling-film evaporator is regulated by a material passing pump through a material regulating valve and then is sent into the second-stage forced circulation evaporator, and the material passing regulating valve is automatically controlled by a liquid level sensor of the second-stage forced circulation evaporator in a linkage manner. After the concentration of the two-stage evaporator is reached, the mixture is conveyed to a crystallizer by a discharge pump, the crystallizer adopts a jacket crystal slurry tank, the crystal slurry tank is cooled by circulating cooling water to separate out crystals, the purposes of thickening and growing the crystals are achieved, and then the crystals enter a centrifugal machine for solid-liquid separation. Discharging borax from a solid discharge port of a centrifugal machine; the liquid discharge port of the centrifuge is communicated with the inlet of the mother liquor tank, and the outlet of the mother liquor tank is respectively communicated with the feed port of the secondary forced circulation evaporator and the discharge device. Most of the mother liquor separated by the centrifuge returns to the evaporator system for further evaporation and concentration, and a small part of the mother liquor is discharged out of the system for treatment through an external discharge device, wherein the external discharge device can be a conveying pipeline or a storage tank. Wherein, when the temperature of the crystallizer is controlled to be above 60 ℃, borax pentahydrate can be crystallized; when the temperature of the crystallizer is controlled below 60 ℃, borax decahydrate can be crystallized.
Furthermore, condensed water outlets of the primary one-effect falling-film evaporator, the primary two-effect falling-film evaporator and the secondary forced circulation evaporator are communicated with an inlet of a condensed water tank, and an outlet of the condensed water tank is communicated with a heat source inlet of the primary preheater and used as a heat source of the primary preheater. Preferably, noncondensable gas outlets of the first-stage one-effect falling-film evaporator, the first-stage two-effect falling-film evaporator and the second-stage forced circulation evaporator are communicated with an inlet of the second-stage preheater and are used as a heat source for the second-stage preheating; the outlet of the condenser is communicated with the inlet of the primary preheater and used as a heat source for primary preheating. The condensed water and the secondary steam generated in the system are fully utilized, the process operation cost is low, the consumption of the condensed water is low, the energy utilization rate is high, and the economic benefit is high.
With reference to the evaporative crystallization process and apparatus for producing borax from the lithium extraction effluent of salt lake provided in the above embodiment 2, the specific steps of the evaporative crystallization process and apparatus for producing borax from the lithium extraction effluent of salt lake provided in the embodiment of the present invention are described as follows:
the first step is as follows: the preheated boron-containing wastewater enters a primary one-effect falling-film evaporator, raw steam (or secondary steam after mechanical compression) is used as a heat source, the heated solution reaches a certain temperature under a specific pressure, water is evaporated to generate secondary steam, and primary one-effect evaporation concentration of materials is carried out to reach a designed concentration;
the second step is that: conveying the material subjected to the primary one-effect evaporation concentration to a primary two-effect falling-film evaporator by a material passing pump, feeding secondary steam generated by the evaporation of the primary one-effect falling-film evaporator as a heating heat source of the primary two-effect falling-film evaporator into the primary two-effect falling-film evaporator, maintaining the pressure of the primary two-effect falling-film evaporator at a specific pressure, allowing the heated solution to reach a certain temperature, evaporating water to generate secondary steam, and performing the primary two-effect evaporation concentration on the material to reach a designed concentration; meanwhile, secondary steam generated by the first-stage two-effect falling-film evaporator enters an MVR steam compressor for compression, and the compressed and heated secondary steam serving as a heat source enters the first-stage one-effect falling-film evaporator and the second-stage forced circulation evaporator to serve as heat sources;
the third step: conveying the material subjected to the primary two-effect evaporation concentration to a secondary forced circulation evaporator by a material passing pump, and performing evaporation concentration by circularly heating by using raw steam (or secondary steam after mechanical compression) as a heat source; a material passing regulating valve is arranged behind the material passing pump, the second-stage forced circulation evaporator is provided with a liquid level sensor, the material passing regulating valve and the liquid level sensor are in linkage automatic control, when the second-stage forced circulation evaporator reaches a set liquid level, the material passing regulating valve is opened, and the material passing pump starts to convey materials;
the fourth step: the material concentrated by the second-stage forced circulation evaporator to reach the designed concentration enters a crystallizer, the crystallizer adopts a jacket crystal slurry tank, and a cooling water is introduced into a jacket of the crystal slurry tank for cooling by circulating cooling water to separate out crystals, so that the aims of thickening and growing the crystals are fulfilled;
the fifth step: conveying the crystal slurry from the crystallizer to a centrifugal machine for solid-liquid separation to separate borax solid; the separated liquid enters a mother liquid tank, most of the mother liquid returns to the secondary forced circulation evaporator to be continuously evaporated, and a small part of the mother liquid is discharged for treatment.
Further, in the first step, the boron-containing wastewater enters the first-stage first-effect falling-film evaporator and the second-stage preheater in sequence for preheating before entering the first-stage first-effect falling-film evaporator, condensed water generated by evaporative concentration of the first-stage first-effect falling-film evaporator, the first-stage second-effect falling-film evaporator and the second-stage forced circulation evaporator and condensed water of the second-stage preheater are recycled and enter the condensed water tank and then enter the first-stage preheater to serve as a heat source for first-stage preheating. The non-condensable gas generated by the evaporation and concentration of the first-stage one-effect falling-film evaporator, the first-stage two-effect falling-film evaporator and the second-stage forced circulation evaporator is recycled and enters the second-stage preheater to be used as a heat source of the second-stage preheater. The condensed water from the secondary preheater enters a condenser, and the generated condensed water enters the primary preheater and is used as a heat source for primary preheating.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "vertical", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and operate, and thus, should not be construed as limiting the present invention.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (13)
1. An evaporative crystallization process for producing borax from a salt lake lithium extraction discharge liquid, which is characterized in that: the concentration section adopts a two-stage MVR combined evaporator to carry out evaporation concentration on the boron-containing wastewater; the crystallization section adopts a cooling crystallization mode to produce borax products; wherein:
the two-stage MVR combined evaporator of the concentration section adopts a combination of a first-stage falling film evaporator and a second-stage forced circulation evaporator; the first-stage falling-film evaporator at least comprises a single-effect falling-film evaporator; or the first-stage falling-film evaporator adopts a mode of connecting two-effect falling-film evaporators in series;
when the two-stage MVR combined evaporator adopts the combination of a one-stage single-effect falling-film evaporator and a two-stage forced circulation evaporator, the concentration mode comprises the following steps:
the preheated boron-containing wastewater enters a first-stage single-effect falling-film evaporator for heating and evaporation, and secondary steam generated by the evaporator enters an MVR steam compressor;
the feed liquid concentrated by the first-stage single-effect falling-film evaporator enters a second-stage forced circulation evaporator to be continuously evaporated and concentrated, and secondary steam generated by the evaporator enters the MVR steam compressor;
the secondary steam compressed by the MVR steam compressor enters the primary single-effect falling-film evaporator and the secondary forced circulation evaporator to be used as heating steam;
the discharge of the secondary forced circulation evaporator enters a crystallizer, and the temperature is reduced and the crystallization is carried out in the crystallizer;
the discharged material of the crystallizer enters a centrifugal machine for solid-liquid separation, and a borax product is separated;
when the two-stage MVR combined evaporator adopts a combination of a first-stage double-effect falling film evaporator and a second-stage forced circulation evaporator, the concentration mode comprises the following steps:
the preheated boron-containing wastewater enters a first-stage one-effect falling-film evaporator for heating and evaporation, secondary steam generated by the evaporator enters a first-stage two-effect falling-film evaporator as a heat source, and the feed liquid concentrated by the first-stage one-effect falling-film evaporator enters the first-stage two-effect falling-film evaporator for heating and evaporation;
the secondary steam generated by the first-stage two-effect falling-film evaporator enters an MVR steam compressor;
the feed liquid concentrated by the first-stage two-effect falling-film evaporator enters a second-stage forced circulation evaporator for evaporation and concentration, and secondary steam generated by the evaporator enters the MVR steam compressor;
the secondary steam compressed by the MVR steam compressor enters the primary one-effect falling-film evaporator and the secondary forced circulation evaporator to be used as heating steam;
the discharge of the secondary forced circulation evaporator enters a crystallizer, and the temperature is reduced and the crystallization is carried out in the crystallizer;
and (4) feeding crystal slurry generated by the crystallizer into a centrifugal machine for solid-liquid separation, and separating a borax product.
2. The evaporative crystallization process for producing borax from a salt lake lithium extraction discharge solution according to claim 1, wherein a primary preheater and a secondary preheater which are connected in sequence are used for preheating boron-containing wastewater, and feed liquid preheated by the secondary preheater enters the primary falling-film evaporator.
3. The evaporative crystallization process for producing borax from salt lake lithium extraction discharge liquid according to claim 2, wherein non-condensable gas generated by the primary falling-film evaporator and the secondary forced circulation evaporator is recycled to enter the secondary preheater for preheating.
4. The evaporative crystallization process for producing borax from a salt lake lithium extraction discharge liquid according to claim 3, wherein condensed water generated by the primary falling-film evaporator, the secondary forced circulation evaporator and the secondary preheater is recycled into a condensed water tank and then enters the primary preheater for preheating.
5. The evaporative crystallization process for producing borax from lithium extraction effluent of salt lake as claimed in claim 4, wherein non-condensable gas generated by the secondary preheater enters a condenser, and condensed water after condensation enters a primary preheater for preheating.
6. The evaporative crystallization process for producing borax from lithium extraction discharge liquid of salt lake according to claim 1, wherein the crystallizer adopts a jacket crystal slurry tank, the crystal slurry tank is cooled by circulating cooling water to separate out crystals in the tank, so as to achieve the purposes of thickening and crystal growing, and then the crystals enter a centrifuge to perform solid-liquid separation.
7. The evaporative crystallization process for producing borax from salt lake lithium extraction discharge liquid according to claim 1, wherein a mother liquid separated by the centrifuge is partially returned to the secondary forced circulation evaporator and partially discharged outside.
8. An evaporation crystallization device for producing borax from a salt lake lithium extraction discharge liquid is characterized in that: the MVR concentration system comprises a first-stage single-effect falling-film evaporator or a first-stage double-effect falling-film evaporator and a second-stage forced circulation evaporator, wherein:
the MVR concentration system composed of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator comprises:
a first-stage single-effect falling-film evaporator;
the discharge port of the primary single-effect falling-film evaporator is connected with the feed port of the secondary forced circulation evaporator;
a vapor inlet of the MVR vapor compressor is connected with vapor outlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator; the vapor outlet of the MVR vapor compressor is connected with the vapor inlets of the first-stage single-effect falling-film evaporator and the second-stage forced circulation evaporator;
the inlet of the crystallizer is connected with the discharge hole of the secondary forced circulation evaporator; the jacket of the crystallizer is connected with a circulating cooling water pipe;
the system comprises a centrifugal machine, a feed inlet of the centrifugal machine is connected with a discharge outlet of the crystallizer, a solid discharge outlet of the centrifugal machine discharges borax, and a liquid discharge outlet of the centrifugal machine is connected with a mother liquor tank;
the MVR concentration system composed of the first-stage double-effect falling-film evaporator and the second-stage forced circulation evaporator comprises:
the primary double-effect falling-film evaporator comprises a primary one-effect falling-film evaporator and a primary two-effect falling-film evaporator, a secondary steam outlet of the primary one-effect falling-film evaporator is connected with a steam inlet of the primary two-effect falling-film evaporator, and a discharge hole of the primary one-effect falling-film evaporator is connected with a feed hole of the primary two-effect falling-film evaporator;
the discharge hole of the first-stage two-effect falling-film evaporator is connected with the feed hole of the second-stage forced circulation evaporator;
a vapor inlet of the MVR vapor compressor is connected with a vapor outlet of the first-stage two-effect falling-film evaporator and a vapor outlet of the second-stage forced circulation evaporator, and a vapor outlet of the MVR vapor compressor is connected with a vapor inlet of the first-stage one-effect falling-film evaporator and a vapor inlet of the second-stage forced circulation evaporator;
the inlet of the crystallizer is connected with the discharge hole of the secondary forced circulation evaporator; the jacket of the crystallizer is connected with a circulating cooling water pipe;
the centrifuge, centrifuge's pan feeding mouth with the discharge gate of crystallizer is connected, centrifuge's solid discharge gate discharge borax, centrifuge's liquid discharge gate is connected with the mother liquor jar.
9. The evaporative crystallization device for producing borax from a salt lake lithium extraction discharge liquid according to claim 8, wherein an outlet of the mother liquid tank is respectively connected with the secondary forced circulation evaporator and an external discharge device.
10. The evaporative crystallization device for producing borax from salt lake lithium extraction effluent as claimed in claim 8, further comprising a primary preheater and a secondary preheater connected, wherein the secondary preheater is connected with a feed inlet of the primary falling film evaporator.
11. The evaporative crystallization device for producing borax from salt lake lithium extraction discharge liquid according to claim 10, wherein the non-condensable gas outlets of the primary falling-film evaporator and the secondary forced circulation evaporator are connected with the inlet of the secondary preheater.
12. The evaporative crystallization device for producing borax from salt lake lithium extraction effluent as claimed in claim 10, wherein the non-condensable gas outlet of the secondary preheater is connected with the inlet of a condenser, and the outlet of the condenser is connected with the inlet of the primary preheater.
13. The evaporative crystallization device for producing borax from a salt lake lithium extraction discharge liquid according to claim 10, wherein condensed water outlets of the primary falling-film evaporator and the secondary forced circulation evaporator are connected with an inlet of a condensed water tank, and an outlet of the condensed water tank is connected with an inlet of the primary preheater.
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| CN114751476A (en) * | 2022-04-21 | 2022-07-15 | 启东神农机械有限公司 | Concentration process of wheat starch slurry and evaporation concentration system thereof |
| CN114949893A (en) * | 2022-06-01 | 2022-08-30 | 启东神农机械有限公司 | Evaporative crystallization process and device for producing lithium chloride from salt lake brine |
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