CN103482657B - Method for concentrating unsaturated salt lake brine at low temperature - Google Patents
Method for concentrating unsaturated salt lake brine at low temperature Download PDFInfo
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- CN103482657B CN103482657B CN201310453093.9A CN201310453093A CN103482657B CN 103482657 B CN103482657 B CN 103482657B CN 201310453093 A CN201310453093 A CN 201310453093A CN 103482657 B CN103482657 B CN 103482657B
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- salt lake
- lake brine
- unsaturated
- concentration
- unsaturated salt
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- 239000012267 brine Substances 0.000 title claims abstract description 65
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000008014 freezing Effects 0.000 claims abstract description 31
- 238000007710 freezing Methods 0.000 claims abstract description 31
- 238000005516 engineering process Methods 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000012141 concentrate Substances 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 description 42
- 241001131796 Botaurus stellaris Species 0.000 description 24
- 229910052736 halogen Inorganic materials 0.000 description 14
- 150000002367 halogens Chemical class 0.000 description 14
- 150000003839 salts Chemical class 0.000 description 9
- 239000000284 extract Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 229910052792 caesium Inorganic materials 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical group [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000002631 hypothermal effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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- Non-Alcoholic Beverages (AREA)
Abstract
The invention discloses a method for concentrating unsaturated salt lake brine at a low temperature. The method is characterized by comprising at least one time of the following freezing concentration step: the unsaturated salt lake brine is placed at a temperature below the freezing point of the unsaturated salt lake brine, so that the surface of the unsaturated salt lake brine is frozen, and concentrated salt lake brine under an ice layer is obtained. A freezing concentration manner is adopted, and low-temperature solubility of a salt-water system is used, so that low-temperature concentration of the unsaturated salt lake brine is realized. According to the method, climate environment energy (such as winter low-temperature cold energy) can be used, the technology is simple and efficient, the cost is low, and energy conservation and environment protection are realized. The technological difficulty that the unsaturated salt lake brine is difficult to evaporate and concentrate in the winter is solved, and the method is particularly suitable for development and utilization of salt lake brine resources in alpine regions of our country.
Description
Technical field
The present invention relates to salt lake brine concentration technology, be specifically related to a kind of method utilizing the unsaturated salt lake brine of cryoconcentration.
Background technology
China has abundant salt lake resources, wherein has its bittern concentration of many salt lakes lighter, does not far reach contained salt saturation ratio, as: Ali Area, Xizang draws the wrong salt lake of fruit, and this kind of salt lake is mainly distributed in the extremely frigid zones in Qinghai and Tibet.In this kind of salt lake being principal character with unsaturated bittern, there are many salt lakes containing enriching the rare and scatter elements such as Li, Rb, Cs.Compared with identical type saturated bittern resource, this type of salt lake brine is after concentrated reaching capacity, and wherein rare and scatter element content is by the content far above identical type saturated bittern resource.
Therefore, need a kind of can with the method for the unsaturated bittern of low cost rapid concentration, with rare and scatter elements such as enrichment Li, Rb, Cs, provide possibility for developing the rare and scatter elements such as Li, Rb, the Cs of high price in this type of salt lake resources.
At present, in exploit resources of salt lakes process, the concentrated method of bittern generally adopts Solar pond production mode.Solar pond production technology utilizes natural energy resources, as: luminous energy, wind energy, cold energy etc., make bittern carry out spontaneous evaporation in salt pond, and in evaporative process, separate out different minerals according to the segmentation of bittern crystallization path, high value rare and scatter element wherein is finally enriched to old halogen.Solar pond production can make the major constituents such as the sylvite in bittern obtain concentrated crystallization; The high value rare and scatter elements such as Li, Rb, Cs obtain enrichment, provide high quality raw material for being processed into finished product further.In the salt lake exploitation at home and abroad of this technology, Application comparison is general, more typically there is magnesium sulfate salt lake salt field process, as: lithium salt field process etc. is carried in the East Platform salt lake of Qinghai Salt Lake institute of Chinese Academy of Sciences exploitation, and chloride type salt lake salt field process, as Cha Er Han Salt Lake salt field process.
Solar pond production technology compares and has superiority in the Salt Lake Area development of resources that steam output is larger, but lower at temperature, that steam output is less extremely frigid zones, its winter temperature is usually less than-10 DEG C, depends merely on Solar pond production and but cannot satisfy the demand.Mainly because the fresh water amount that unsaturated salt lake brine will evaporate is very large, and the evaporation periods of needs can be very long, and the cost of Solar pond production can be very high.Therefore, also need one can at lower cost, the temperature environment below-10 DEG C concentrates the method for unsaturated salt lake brine, can make full use of the salt lake resources of China's extremely frigid zones.
Summary of the invention
The present invention is intended at least solve one of above-mentioned problem, provides a kind of method that the mode of freezing can be utilized to concentrate unsaturated bittern.
Technical scheme of the present invention is the method for the unsaturated salt lake brine of a kind of cryoconcentration, comprise Freeze Concentration step following at least one times: described unsaturated salt lake brine is placed in its temperature below freezing, to make its surface freeze, obtain the concentrated salt lake brine under ice sheet.
Preferably, described method comprises three described Freeze Concentration steps.
In some embodiments, described temperature below freezing can be less than-5 DEG C, is preferably less than-10 DEG C.
In some embodiments, the thickness of described unsaturated salt lake brine can be more than 30cm, is preferably more than 40cm.
In some embodiments, the thickness of described ice sheet can be more than 10cm, is preferably more than 15cm.
In some embodiments, described temperature below freezing can utilize natural climate environment to reach.
In some embodiments, in described concentrated salt lake brine, the concentration of rare and scatter element can be more than 3.0 times of rare and scatter element concentration described in original unsaturated salt lake brine.
The present invention adopts freeze concentration mode, utilizes the dissolution in low temperature character of salt-water system, achieves the cryoconcentration of unsaturated salt lake brine.The method can utilize the climatope energy (such as, winter low temperature cold energy), and technique is simply efficient, with low cost, energy-conserving and environment-protective.Solve the technical bottleneck of unsaturated bittern evaporation concentration in winter difficulty, be especially applicable to the development and utilization of the extremely frigid zones salt lake brine resource of China.
Embodiment
According to Na under low temperature
+, K
+//Cl
-, SO
4 2--H
2o quaternary salt-water system, Na
+, K
+, Mg
2+//Cl
-, SO
4 2--H
2the dissolubility data of O quinary system, brine temperature be in its below freezing time, bittern will tie pure ice.The freezing point of unsaturated bittern generally more than-10 DEG C, and is rich in the extremely frigid zones of salt lake brine resource in China, winter temperature is all lower than this freezing point, and therefore, the mode be very beneficial for by freezing realizes the concentrated of salt lake brine.
Particularly, the method of the unsaturated salt lake brine of the cryoconcentration that the present invention relates to, Freeze Concentration step at least one times can be comprised, described freezing concentration step operation is as follows: described unsaturated salt lake brine is placed in its temperature below freezing, to make its surface freeze, obtain the concentrated salt lake brine under ice sheet.
Such as when being rich in the extremely frigid zones of salt lake brine resource for China, can in the winter time hypothermic phase (period below unsaturated salt lake brine freezing point temperature) arrive before, unsaturated salt lake brine is placed in concentration basin, time below the freezing point temperature that temperature enters described unsaturated salt lake brine, to freeze from surface, obtain under ice sheet through concentrated concentrated brine.
Along with the increase gradually of icing thickness, cold energy transmission slows down, and icing rate is slack-off.Therefore, consider from the angle of efficiency and cost, this Freeze Concentration step can be made to repeat repeatedly, with by multistage concentrated, never remove a large amount of fresh water in saturated salt lake bittern water, reach the object of rapidly and efficiently concentrated brine.
Operation can such as particularly, and unsaturated salt lake brine can be made experience for the first time after Freeze Concentration in first step concentration basin, extracts out, pour into bottom the concentration basin of primary concentration bittern from ice sheet second stage concentration basin, carry out second time Freeze Concentration.Similarly, carry out three times, or more time Freeze Concentration.In a preferred embodiment of the invention, three Freeze Concentration steps can being carried out, realizing the concentrated effect to there being valency ionic concn more than 3.0 times in unsaturated salt lake brine.
When comprising repeatedly Freeze Concentration step, usually in third time and concentration process afterwards, may separate out sodium sulfate salt solid (being such as sal glauberi), under it may be bonded at ice sheet, or part is separated out bottom concentration basin simultaneously.However, it should be understood that the precipitation of sal glauberi does not have substantial effect to method of the present invention, therefore also without the need to controlling it.And in fact, the precipitation of sodium sulfate salt to other the main rare and scatter elements in salt lake brine, the enrichment of ion in concentrated brine of such as K, Li, B, Br, Rb, Cs etc. is favourable.
The freezing point temperature of unsaturated salt lake brine is generally at about-5 DEG C, and therefore, this Freeze Concentration step can be carried out below-5 DEG C.In preferred embodiment herein, Freeze Concentration step can the temperature below-10 DEG C be carried out, and can realize the cycles of concentration of more than 3.5 times.Lower temperature is more conducive to improving thickening efficiency.China's extremely frigid zones salt lake brine resource location winter temperature, usually all below-10 DEG C, is applicable to using method of the present invention, utilizes the cryogenic cold energy of natural climate in winter, concentrated unsaturated salt lake brine very much.
Such as consider from the efficiency of Freeze Concentration and cost angle, in concentration basin, the thickness of unsaturated salt lake brine can at more than 30cm, preferably at more than 40cm; In Freeze Concentration process, unsaturated salt lake brine surface ice layer thickness at more than 10cm, can be preferably more than 15cm.After multistage Freeze Concentration, when concentrated brine concentration reaches capacity, bittern freezing point is equal to or less than temperature, obtain final concentrated brine.
The present invention make use of the feature that unsaturated bittern freezes at low temperatures dexterously, utilizes extremely frigid zones winter low temperature cold energy residing for salt lake, removes fresh water a large amount of in unsaturated salt lake brine, reach the object of rapidly and efficiently concentrated brine by the mode of freezing.Technique is simple, with low cost, energy-conserving and environment-protective.Not only solve the technical bottleneck of unsaturated bittern evaporation concentration in winter difficulty, be also especially applicable to the development and utilization of the extremely frigid zones salt lake brine resource of China.
By the technology of the present invention, utilize the period in a short winter, can reach capacity unsaturated salt lake brine concentration state, has the concentration of valency ion to improve at least more than 3-4 times in bittern.Respectively there is the concentration of valency ion and rare and scatter element can improve 3-4 doubly in final concentrated brine, such as, can reach more than 3.5 times of former halogen content.Generally, concentrated 3-4 times of rear bittern concentration can reach commercial exploitation grade.
In addition, method of the present invention can also with common evaporation salt pan concentration technique combined utilization, to freeze on enriched basic, then through Solar pond production, to improve the commercial exploitation grade of salt lake brine further, fully this type of salt lake resources of exploitation.
Draw the concentrated as example of the wrong salt lake brine of fruit below using Tibet, in conjunction with specific embodiments the present invention is described in further detail.
The one-tenth that following table is listed in raw material salt lake bittern water is grouped into.
Embodiment 1
1st grade of Freeze Concentration: by former for 100t halogen (volume 92.59m
3) be placed in 1 grade of concentration basin, controlling bittern thickness is 400 ± 20mm, in temperature lower than-10 DEG C of environment, carries out Freeze Concentration.When ice layer thickness reaches 15cm, the 1st grade has concentrated, has obtained the liquid phase A below ice sheet.
The volume of liquid phase A is 60.6m
3, concentrated about 1.5 times of more former halogen, its one-tenth is grouped into the 1-1 that sees the following form.
The one-tenth of table 1-1 liquid phase A is grouped into
2nd grade of Freeze Concentration: extract liquid phase A out bottom 1 grade of concentration basin, is placed in 2 grades of concentration basins, freezing liquid phase A under the condition of envrionment temperature lower than-10 DEG C, and when freezing layer thickness and reaching 15cm, the 2nd grade has concentrated, obtained the liquid phase B below ice sheet.
The volume of liquid phase B is 40.8m
3, concentrated about 2.2 times of more former halogen, its one-tenth is grouped into the 1-2 that sees the following form.
The one-tenth of table 1-2 liquid phase B is grouped into
3rd level Freeze Concentration: extract liquid phase B out bottom 2 grades of concentration basins, be placed in 3 grades of concentration basins, freezing liquid phase B under the condition of envrionment temperature lower than-10 DEG C, when ice layer thickness reaches 15cm, 3rd level has concentrated, and obtains the liquid phase C below ice sheet.The sal glauberi solid of about 2.8t is separated out in concentrating for this time.
Liquid phase C volume 25.5m
3, concentrated about 3.6 times of more former halogen, its one-tenth is grouped into the 1-3 that sees the following form.
The one-tenth of table 1-3 liquid phase C is grouped into
After three grades of freeze concentration, being separated and obtaining liquid phase volume is 25.5m
3, weight is 30.5t, and wherein leading ion cycles of concentration is all more than 3.5 times.
Embodiment 2
First step Freeze Concentration: by former for 100t halogen (volume 92.59m
3) be placed in 1 grade of concentration basin, controlling bittern thickness is 400 ± 20mm, in temperature lower than in-10 DEG C of environment, carries out Freeze Concentration.When ice layer thickness reaches 15cm, the 1st grade has concentrated, has obtained the liquid phase A below ice sheet.
The volume of liquid phase A is 60.4m
3, concentrated about 1.5 times of more former halogen, its one-tenth is grouped into the 2-1 that sees the following form.
The one-tenth of table 2-1 liquid phase A is grouped into
2nd grade of Freeze Concentration: extract liquid phase A out bottom 1 grade of concentration basin, is placed in 2 grades of concentration basins, freezing liquid phase A under the condition of envrionment temperature lower than-10 DEG C, and when freezing layer thickness and reaching 15cm, 2 grades have concentrated, obtained liquid phase B.
The volume of liquid phase B is 41.2m
3, concentrated about 2.2 times of more former halogen, its one-tenth is grouped into the 2-2 that sees the following form.
The one-tenth of table 2-2 liquid phase B is grouped into
3rd level Freeze Concentration: extract liquid phase B out bottom 2 grades of concentration basins, is placed in 3 grades of concentration basins, freezing liquid phase B under the condition of envrionment temperature lower than-10 DEG C, and when ice layer thickness reaches 15cm, 3 grades have concentrated, obtained liquid phase C.
The volume of liquid phase C is 26.1m
3, concentrated about 3.5 times of more former halogen, its one-tenth is grouped into the 2-3 that sees the following form.
The one-tenth of table 2-3 liquid phase C is grouped into
After three grades of freeze concentration, being separated and obtaining liquid phase volume is 26.1m
3, weight is 31.3t, and wherein leading ion cycles of concentration is all more than 3.5 times.
Embodiment 3
1st grade of Freeze Concentration: by former for 100t halogen (volume 92.59m
3) be placed in 1 grade of concentration basin, controlling bittern thickness is 400 ± 20mm, in temperature lower than in-10 DEG C of environment, carries out Freeze Concentration.When ice layer thickness reaches 15cm, the 1st grade has concentrated, has obtained the liquid phase A below ice sheet.
The volume of liquid phase A is 62.6m
3, concentrated about 1.5 times of more former halogen, its one-tenth is grouped into the 3-1 that sees the following form.
The one-tenth of table 3-1 liquid phase A is grouped into
2nd grade of Freeze Concentration: extract liquid phase A out bottom 1 grade of concentration basin, is placed in 2 grades of concentration basins, freezing liquid phase A under the condition of envrionment temperature lower than-10 DEG C, and when freezing layer thickness and reaching 15cm, 2 grades have concentrated, obtained liquid phase B.
The volume of liquid phase B is 41.0m
3, concentrated about 2.2 times of more former halogen, its one-tenth is grouped into the 3-2 that sees the following form.
The one-tenth of table 3-2 liquid phase B is grouped into
3rd level Freeze Concentration: extract liquid phase B out bottom 2 grades of concentration basins, is placed in 3 grades of concentration basins, freezing liquid phase B under the condition of envrionment temperature lower than-10 DEG C, and when ice layer thickness reaches 15cm, 3 grades have concentrated, obtained liquid phase C.
The volume of liquid phase C is 22.3m
3, concentrated about 4.0 times of more former halogen, its one-tenth is grouped into the 3-3 that sees the following form.
The one-tenth of table 3-3 liquid phase C is grouped into
After three grades of freeze concentration, being separated and obtaining liquid phase volume is 22.3m
3, weight is 26.7t, and wherein leading ion cycles of concentration is all more than 3.5 times.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Any various other done by technical conceive of the present invention change and distortion accordingly, all should be included in the protection domain of the claims in the present invention.
Claims (6)
1. the method for the unsaturated salt lake brine of cryoconcentration, it is characterized in that, described method comprises Freeze Concentration step following at least one times: described unsaturated salt lake brine is placed in its temperature below freezing, freeze to make its surface, obtain the concentrated salt lake brine under ice sheet, and described method does not comprise Exposure to Sunlight enrichment step, wherein
Described temperature below freezing is less than-5 DEG C, the thickness of described unsaturated salt lake brine is more than 30cm, the thickness of described ice sheet is more than 10cm, has the concentration of valency ion for there being more than 3.0 times of valency ionic concn described in original unsaturated salt lake brine in described concentrated salt lake brine.
2. the method for the unsaturated salt lake brine of cryoconcentration as claimed in claim 1, wherein, described method comprises three described Freeze Concentration steps.
3. the method for the unsaturated salt lake brine of cryoconcentration as claimed in claim 1, wherein, described temperature below freezing is less than-10 DEG C.
4. the method for the unsaturated salt lake brine of cryoconcentration as claimed in claim 1, wherein, the thickness of described unsaturated salt lake brine is more than 40cm.
5. the method for the unsaturated salt lake brine of cryoconcentration as claimed in claim 1, wherein, the thickness of described ice sheet is more than 15cm.
6. the method for the unsaturated salt lake brine of cryoconcentration as claimed in claim 1, wherein, described temperature below freezing utilizes natural climate environment to reach.
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| CN108421277A (en) * | 2018-04-04 | 2018-08-21 | 清华大学 | A method of the system and its enrichment salt lake bittern of enrichment salt lake bittern |
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