CN115010150B - MVR thermal method nitrate extraction process - Google Patents
MVR thermal method nitrate extraction process Download PDFInfo
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- CN115010150B CN115010150B CN202210470057.2A CN202210470057A CN115010150B CN 115010150 B CN115010150 B CN 115010150B CN 202210470057 A CN202210470057 A CN 202210470057A CN 115010150 B CN115010150 B CN 115010150B
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- China
- Prior art keywords
- salt
- tank
- nitrate
- evaporation tank
- washer
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- 229910002651 NO3 Inorganic materials 0.000 title claims abstract description 47
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000000605 extraction Methods 0.000 title claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 97
- 238000001704 evaporation Methods 0.000 claims abstract description 39
- 230000008020 evaporation Effects 0.000 claims abstract description 39
- 239000012267 brine Substances 0.000 claims abstract description 36
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000005185 salting out Methods 0.000 claims abstract description 5
- 230000018044 dehydration Effects 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims description 5
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007832 Na2SO4 Substances 0.000 abstract 1
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract 1
- 235000011152 sodium sulphate Nutrition 0.000 abstract 1
- 239000010446 mirabilite Substances 0.000 description 8
- 239000012452 mother liquor Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 241001131796 Botaurus stellaris Species 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002828 nitro derivatives Chemical class 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a salt making process method, in particular to an MVR thermal method nitrate extraction process in a salt making process, and belongs to the technical field of chemical industry. Raw brine or refined brine of the invention sequentially enters a salt evaporation tank 210 and 210 after being preheated and heated, salt slurry generated by the salt evaporation tank 210 is discharged to a salt collecting box, washed by a salt washer, centrifugally dehydrated and dried, and secondary steam generated by the salt evaporation tank 210 enters the salt evaporation tank 210 again after being washed by a steam washer and compressed by a compressor; the old brine after salt washing by the salt washer is removed from the settler, clear liquid of the settler is preheated and heated and enters a nitrate tank 310 for salting out and separating out nitrate, salt and nitrate mud at the bottom of the settler are also pumped into the nitrate tank 310, nitrate slurry in the nitrate tank 310 is removed for centrifugal dehydration and drying, and clear liquid is transferred to a salt evaporation tank 210. The invention can co-produce high-quality salt and Na2SO4, has high heat efficiency and greatly saves production cost.
Description
Technical Field
The invention relates to a salt making process method, in particular to an MVR thermal method nitrate extraction process in a salt making process, and belongs to the technical field of chemical industry.
Background
The domestic mine salt brine type is mainly mirabilite type brine, but the mirabilite type brine is generally high in Na 2SO4 content, is not economical to remove by a chemical method, and cannot be considered. Therefore, the production process of mirabilite type brine mainly comprises two types: firstly, traditional multiple-effect evaporation guarantees salt quality through a mode of discharging a large amount of mother liquor or discharging old brine after salt washing, but the method has low heat utilization rate, low salt quality and serious waste of nitrate resources. Secondly, the process of salt and nitrate co-production (also called as a mother liquor recovery method) introduced from abroad in nineties of the last century has the advantages of high resource utilization rate, good product quality and high degree of automation, but when the Na 2SO4 content is high, the yield proportion of a salt system with high heat utilization rate is reduced, the yield proportion of a salt and nitrate separation system with high energy consumption is increased, so that the comprehensive energy consumption of the whole device is rapidly increased along with the increase of the Na 2SO4 content, and the process has the advantages of brine purification, further increased cost and low competitiveness in a high-quality and non-optimal market large environment. For this reason, it is necessary to explore energy-saving processes for high-nitrate brine.
In recent years, MVR has been using a foreign army protrusion with the progress of national environmental policy and the adjustment of energy structure. MVR is a short term of mechanical vapor recompression technology (MECHANICAL VAPOR RECOMPRESSION), which uses the secondary vapor and energy thereof generated by the evaporation system itself to promote the low-grade vapor to be a high-grade vapor heat source through the mechanical work of the compressor. The circulation provides heat energy for the evaporation system, so that the energy saving technology reduces the demand for external energy, and the energy saving technology is a heating system which saves primary energy most in the world at present. During multi-effect evaporation, secondary steam generated by end effect contains a large amount of heat, but cannot be utilized due to low temperature, and a large amount of cooling water is required to be consumed for condensation, so that the improvement of heat efficiency is limited. The heat pump is used for boosting and heating the low-temperature secondary steam through mechanical compression and recycling, so that the defect that a large amount of heat energy of the final-effect secondary steam cannot be utilized is overcome, the comprehensive energy consumption is extremely low, and the primary energy utilization rate of the optimally designed mechanical compression heat pump is higher than that of eight-effect evaporation. The application of heat pumps is also limited by a number of factors. Firstly, the investment is large, and the more effective evaporation is generally higher than 10% (the investment can be greatly reduced if the compressor of key equipment is made in China). And secondly, the constraint of energy price. The compression heat pump is based on the premise of consuming a certain amount of electric energy, the application of the heat pump is greatly affected by the specific value of the electric energy and the fuel, and the application prospect of the heat pump is bright along with the gradual reduction and exhaustion of fossil energy. There are now more direct steam driven technologies that are more thermally efficient due to reduced waste of thermoelectric conversion. Thirdly, the influence of raw material brine. For gypsum type brine, after the brine is purified, the impurity content in the brine is very small except NaCl, and a large amount of mother liquor is not required to be discharged, so that the thermal efficiency is very high; for mirabilite brine, since the refined brine also contains more Na 2SO4, a salt and nitrate separation system is necessary. Because the salt and nitrate separation system consumes higher, the thermal efficiency of the whole device is reduced, and the higher the content of mirabilite in brine is, the more mother liquor is discharged from the salt system, the larger the proportion of the salt and nitrate separation system is, and the lower the thermal efficiency of the whole device is.
The thermal method is a process for extracting nitro-compound developed in the early 80 s of the last century in China, and also utilizes the reverse dissolution characteristic of Na 2SO4 at more than 17.9 ℃ to heat the high-nitro-compound bittern discharged from salt preparation to about 100 ℃, and adds powder salt into the preheated bittern or enters a nitro-compound evaporation tank to evaporate and concentrate (so-called salting-out method) so that the old bittern which is unsaturated by NaCI after heating becomes saturated solution or nearly saturated solution, the Na 2SO4 is separated out due to the homoionic effect of Na +, and the mother liquor after the nitro-compound extraction is sent back to a salt preparation system to produce salt.
The method is characterized in that: the heat efficiency is higher, the waste heat of condensed water is recovered, secondary steam is extracted for preheating, the steam utilization rate is improved, the salt removal concentration is high, and the heat loss is small; the process flow for producing anhydrous mirabilite is short, brine is not purified, investment is saved, brine is circulated in a closed mode, mother liquor is not discharged, and the brine consumption for preparing salt and the pollution to the environment can be reduced. The disadvantages are: the quality of salt is low, the quality of nitrate is poor, because calcium and magnesium impurities in brine are not removed, partial calcium and magnesium impurities enter a nitrate tank, and because the calcium and magnesium impurities enter mirabilite, the salt is difficult to remove by a washing method, the quality of the nitrate can only reach about 95 percent or even lower, and the commercial value is low. Therefore, the process cannot be popularized, and only the salinization of the blue sky persists for many years. The thermal method for extracting the nitrate has the advantages of low investment and high heat utilization rate, and solves the aeipathia with low product quality, thus being urgent. From the analysis of the principle and the operation process, the salt washing process requires the old brine Na 2SO4 to be as high as possible, even up to more than 70g/l, which has an inevitable effect on the salt quality and is difficult to solve the contradiction. In addition, the process does not adopt brine purification, calcium and magnesium impurities have great influence on the quality of products, and if purification treatment is adopted, the quality of the products, particularly the quality of anhydrous nitrate, is inevitably improved greatly. But this in turn increases investment and operating costs.
In recent years, with the great drop of mirabilite price and the great increase of fuel price, the defect of high consumption of the salt and nitrate co-production process at once in a popular time is developed gradually, and particularly the production of high-nitrate brine has high steam consumption. During death, some enterprises optimize and perfect the processes such as the combined production of the abandoned salt and the nitrate after the death, so that the hot method nitrate extraction process is reselected, which is a technical problem which needs to be solved urgently in the salt production industry.
Disclosure of Invention
The invention aims to solve the technical problem of low heat efficiency in the prior art and provides an MVR thermal method nitrate extraction process.
The invention comprises the following steps: an MVR thermal method nitrate extraction process comprises the following steps: raw brine or refined brine sequentially enters a salt evaporation tank 210 and a salt slurry generated by the salt evaporation tank 210 after being preheated and heated is discharged to a salt collecting tank, is washed by a salt washer and then is centrifugally dehydrated and dried, and secondary steam generated by the salt evaporation tank 210 is compressed by a steam washer and a compressor and then enters the salt evaporation tank 210 again; the old brine after salt washing by the salt washer is removed from the settler, clear liquid of the settler is preheated and heated and enters a nitrate tank 310 for salting out and separating out nitrate, salt and nitrate mud at the bottom of the settler are also pumped into the nitrate tank 310, nitrate slurry in the nitrate tank 310 is removed for centrifugal dehydration and drying, and clear liquid is transferred to a salt evaporation tank 210.
The invention is realized by a device which comprises a salt evaporation tank 210, a salt collecting box, a salt washer, a centrifugal dehydrator and a dryer which are sequentially connected through pipelines, wherein the old brine outlet of the salt washer is connected to a settler through a pipeline, the clear liquid outlet of the settler is connected with the inlet of a nitro-tank 310 through a pipeline, the outlets of salt and nitro-mud at the bottom of the settler are connected with the inlet of the nitro-tank 310 through a pump and a pipeline, the nitro-discharging outlet of the nitro-tank 310 is connected to the centrifugal dehydrator and the nitro-dryer through a pipeline, the feed liquid outlet of the nitro-tank 310 is connected with the feed liquid inlet of the salt evaporation tank 210 through a pipeline, the outlet of secondary steam of the salt evaporation tank 210 is connected with the inlet of a pipeline steam washer, the outlet of the steam washer is connected with the air inlet of a compressor through a pipeline, and the air outlet of the compressor is connected with the steam inlet of the salt evaporation tank 210 through a pipeline.
The invention can co-produce high-quality salt and Na 2SO4, has high heat efficiency and greatly saves production cost.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present invention.
Detailed Description
The invention will now be described in further detail with reference to the drawings and to specific examples.
As shown in fig. 1, the present invention includes the steps of: raw brine or refined brine sequentially enters a salt evaporation tank 210 and a salt slurry generated by the salt evaporation tank 210 after being preheated and heated is discharged to a salt collecting tank, is washed by a salt washer and then is centrifugally dehydrated and dried, and secondary steam generated by the salt evaporation tank 210 is compressed by a steam washer and a compressor and then enters the salt evaporation tank 210 again; the old brine after salt washing by the salt washer is removed from the settler, clear liquid of the settler is preheated and heated and enters a nitrate tank 310 for salting out and separating out nitrate, salt and nitrate mud at the bottom of the settler are also pumped into the nitrate tank 310, nitrate slurry in the nitrate tank 310 is removed for centrifugal dehydration and drying, and clear liquid is transferred to a salt evaporation tank 210.
The invention is realized by a device which comprises a salt evaporation tank 210, a salt collecting box, a salt washer, a centrifugal dehydrator and a dryer which are sequentially connected through pipelines, wherein the old brine outlet of the salt washer is connected to a settler through a pipeline, the clear liquid outlet of the settler is connected with the inlet of a nitro-tank 310 through a pipeline, the outlets of salt and nitro-mud at the bottom of the settler are connected with the inlet of the nitro-tank 310 through a pump and a pipeline, the nitro-discharging outlet of the nitro-tank 310 is connected to the centrifugal dehydrator and the nitro-dryer through a pipeline, the feed liquid outlet of the nitro-tank 310 is connected with the feed liquid inlet of the salt evaporation tank 210 through a pipeline, the outlet of secondary steam of the salt evaporation tank 210 is connected with the inlet of a pipeline steam washer, the outlet of the steam washer is connected with the air inlet of a compressor through a pipeline, and the air outlet of the compressor is connected with the steam inlet of the salt evaporation tank 210 through a pipeline.
The invention saves more than 400 ten thousand yuan of energy cost on the basis of the original production scale (60 ten thousand tons/year), and greatly improves the economic benefit.
Claims (1)
1. An MVR thermal method nitrate extraction process comprises the following steps: raw brine or refined brine sequentially enters a salt evaporation tank 210 and a salt slurry generated by the salt evaporation tank 210 after being preheated and heated is discharged to a salt collecting tank, is washed by a salt washer and then is centrifugally dehydrated and dried, and secondary steam generated by the salt evaporation tank 210 is compressed by a steam washer and a compressor and then enters the salt evaporation tank 210 again; the old brine after being washed by the salt washer is removed from the settler, clear liquid of the settler is preheated and heated and enters a nitrate tank 310 for salting out and separating out nitrate, salt and nitrate mud at the bottom of the settler are also pumped into the nitrate tank 310, nitrate slurry in the nitrate tank 310 is removed for centrifugal dehydration and drying, and clear liquid is transferred to a salt evaporation tank 210; the device comprises a salt evaporation tank 210, a salt collecting box, a salt washer, a centrifugal dehydrator and a dryer which are sequentially connected through pipelines, wherein a old brine outlet of the salt washer is connected to a settler through a pipeline, a clear liquid outlet of the settler is connected with an inlet of a nitro-tank 310 through a pipeline, a bottom salt and nitro-mud outlet of the settler is connected with an inlet of the nitro-tank 310 through a pump and a pipeline, a nitro-discharging outlet of the nitro-tank 310 is connected to the centrifugal dehydrator and the nitro dryer through a pipeline, a feed liquid outlet of the nitro-tank 310 is connected with a feed liquid inlet of the salt evaporation tank 210 through a pipeline, a secondary steam outlet of the salt evaporation tank 210 is connected with an inlet of a steam washer through a pipeline, and a gas outlet of the steam washer is connected with a steam inlet of the salt evaporation tank 210 through a pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210470057.2A CN115010150B (en) | 2022-04-28 | 2022-04-28 | MVR thermal method nitrate extraction process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210470057.2A CN115010150B (en) | 2022-04-28 | 2022-04-28 | MVR thermal method nitrate extraction process |
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| Publication Number | Publication Date |
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| CN115010150A CN115010150A (en) | 2022-09-06 |
| CN115010150B true CN115010150B (en) | 2024-04-26 |
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| CN202210470057.2A Active CN115010150B (en) | 2022-04-28 | 2022-04-28 | MVR thermal method nitrate extraction process |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115607987A (en) * | 2022-10-17 | 2023-01-17 | 中盐长江盐化有限公司 | Seven-effect vacuum salt making process |
| CN115636426A (en) * | 2022-10-27 | 2023-01-24 | 中盐长江盐化有限公司 | Nitrate extraction process by six-effect thermal method |
| CN115557518A (en) * | 2022-10-31 | 2023-01-03 | 孝感广盐华源制盐有限公司 | Method for salt-nitrate co-production through six-effect TVR evaporation glauberite double salt separation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146434A (en) * | 2021-11-15 | 2022-03-08 | 四川西秦盐化科技有限公司 | Process transformation method based on existing multi-effect evaporation salt and nitrate preparation system |
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- 2022-04-28 CN CN202210470057.2A patent/CN115010150B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114146434A (en) * | 2021-11-15 | 2022-03-08 | 四川西秦盐化科技有限公司 | Process transformation method based on existing multi-effect evaporation salt and nitrate preparation system |
Non-Patent Citations (1)
| Title |
|---|
| "母液回收法盐硝联产新工艺";姚立勇;《盐业与化工》;第20-23页 * |
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| CN115010150A (en) | 2022-09-06 |
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