CN112707414A - Method for removing bromine from high-salinity wastewater - Google Patents
Method for removing bromine from high-salinity wastewater Download PDFInfo
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- CN112707414A CN112707414A CN202011482737.3A CN202011482737A CN112707414A CN 112707414 A CN112707414 A CN 112707414A CN 202011482737 A CN202011482737 A CN 202011482737A CN 112707414 A CN112707414 A CN 112707414A
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 89
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 87
- 239000002351 wastewater Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 25
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 38
- 238000004821 distillation Methods 0.000 claims abstract description 26
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 25
- 239000011780 sodium chloride Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 12
- 239000001103 potassium chloride Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000012452 mother liquor Substances 0.000 claims description 39
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 claims description 21
- 235000002639 sodium chloride Nutrition 0.000 claims description 20
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000460 chlorine Substances 0.000 claims description 8
- 229910052801 chlorine Inorganic materials 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000001256 steam distillation Methods 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 3
- BSKZDJXVMPWPRA-UHFFFAOYSA-N O.[Br] Chemical compound O.[Br] BSKZDJXVMPWPRA-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims 3
- 239000002912 waste gas Substances 0.000 claims 1
- 238000003723 Smelting Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000012267 brine Substances 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/096—Bromine
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- 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
-
- 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
- C02F1/10—Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
-
- 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
- C02F2101/12—Halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a method for removing bromine from high-salinity wastewater, which comprises the steps of firstly recovering sodium chloride and potassium chloride in the wastewater by adopting a process of combining multi-effect evaporative crystallization of sodium chloride with cooling crystallization of potassium chloride, and then carrying out distillation and bromine extraction by using water vapor, so that the sodium chloride, the potassium chloride and bromine in the wastewater can be recovered to the maximum extent, zero discharge of smelting wastewater is realized, and environmental pollution is reduced.
Description
Technical Field
The invention relates to the technical field of smelting, in particular to a treatment technology of high salt and bromine content after metal smoke dust is generated by calcining smelting waste residues at high temperature, leaching, dechlorination and valuable metal extraction are carried out, and heavy metal is further recovered from raffinate.
Background
With the improvement of the national environmental protection standard, the smelting wastewater must realize zero emission, and the prior smelting wastewater treatment technology is to perform concentration again through a pretreatment system, and finally evaporate the concentrated solution into sodium sulfate, sodium chloride and potassium chloride salt, so that bromine is not recovered, bromine resource waste is caused, and the environment is further polluted.
Bromine is an important chemical raw material and is widely applied to the fields of high-efficiency combustion improvers, refrigerants, petroleum completion fluids, medicines, fuel intermediates and chemical reagents. At present, the methods for extracting bromine from brine mainly comprise the following four methods:
(1) a distillation method: the method is suitable for brine with bromine content of more than 2g/l, and has narrow application range;
(2) air blown lye absorption method: the method has stable process, high power consumption and large acid and alkali consumption, and is suitable for occasions with sufficient electric power and cheap waste acid and waste alkali;
(3) air blown sulfur dioxide absorption: the method has advanced treatment process, the extraction rate of bromine can reach 70% -80%, but after bromine is extracted from brine for one time, the wastewater is discharged, and the contained bromine cannot be recovered, thereby causing bromine resource waste.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for removing bromine from high-salinity wastewater.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for removing bromine from high-salinity wastewater comprises the following steps:
s1, salt separation evaporation crystallization:
s1.1, preheating bromine-containing high-salinity wastewater, then sending the wastewater into a two-effect evaporator for primary concentration, and then sending the wastewater into a three-effect evaporator for secondary concentration; the preheating temperature is 80-85 ℃;
s1.2, feeding the high-salinity wastewater subjected to secondary concentration into a one-effect evaporator to crystallize to obtain sodium chloride, centrifuging by using a centrifugal machine to obtain sodium chloride and sodium chloride mother liquor, and returning the sodium chloride mother liquor to the one-effect evaporator; sending the evaporation concentrated solution generated in the first-effect evaporator into a cooling crystallizer for crystallization to obtain potassium chloride, and separating the potassium chloride and mother liquor by a centrifugal machine; returning part of the mother liquor to the single-effect evaporator, taking part of the mother liquor as discharged mother liquor to perform bromine enrichment, and entering step S2 when the bromine in the discharged mother liquor is enriched to 2 g/L;
s2, extracting bromine by steam distillation:
s2.1, pumping the discharged mother liquor subjected to bromine enrichment in the step S1.2 into a high-level tank, feeding the discharged mother liquor into a preheater by utilizing level difference, feeding the preheated discharged mother liquor into a distillation tower from the top of the distillation tower, carrying out an oxidation reaction of chlorine and a steam distillation process of free bromine in the distillation tower, and discharging the mother liquor from the bottom of the distillation tower after the reaction is finished; introducing water vapor from the bottom of the distillation tower, and introducing chlorine from the middle section of the distillation tower; the preheating temperature is 60-65 ℃;
s2.2, discharging bromine steam and part of water vapor distilled by the water vapor from the top of the distillation tower into a condenser, condensing the bromine steam and part of the water vapor into crude bromine and bromine water through heat exchange with cooling water in the condenser, and sending the crude bromine and the bromine water into a bromine-water separation bottle; the uncondensed bromine vapor, water vapor and a small amount of chlorine gas enter an absorption tower, and exhaust gas is exhausted after absorption by discharged mother liquor;
s2.3, separating bromine and bromine water in a bromine water separation bottle by utilizing the difference of the gravities of the bromine and the bromine water, returning the bromine water to a distillation tower for redistillation, and rectifying crude bromine in a rectifying tower; after the crude bromine is rectified, refined bromine discharged from the bottom of the rectifying tower enters a cooler for cooling, and then is put into a bromine storage bottle, and the finished bromine is obtained after the bromine storage bottle is packaged by a porcelain jar.
Further, in step S1.1, the bromine-containing high-salinity wastewater may be preheated with non-condensable gas.
Further, in step S2.3, the crude bromine is rectified twice through a primary rectifying tower and a secondary rectifying tower in sequence.
Further, in step S2.3, the tail gas generated in the rectifying tower enters the absorption tower, and the exhaust gas is evacuated after absorption by the discharged mother liquor.
The invention has the beneficial effects that: the invention adopts the process of combining the multi-effect evaporative crystallization of sodium chloride with the cooling crystallization of potassium chloride to firstly recover the sodium chloride and the potassium chloride in the wastewater, and then utilizes the steam to distill and extract bromine, thereby being capable of recovering the sodium chloride, the potassium chloride and the bromine in the wastewater to the maximum extent, realizing zero discharge of the smelting wastewater and reducing the environmental pollution.
Drawings
FIG. 1 is a flowchart illustrating step S1 according to an embodiment of the present invention;
fig. 2 is a flowchart illustrating step S2 according to an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that the present embodiment is based on the technical solution, and the detailed implementation and the specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
The embodiment provides a method for removing bromine from high-salinity wastewater, which comprises the following steps:
s1, salt separation, evaporation and crystallization, as shown in figure 1:
s1.1, preheating bromine-containing high-salinity wastewater, then sending the wastewater into a two-effect evaporator for primary concentration, and then sending the wastewater into a three-effect evaporator for secondary concentration; the preheating temperature is 80-85 ℃;
in this embodiment, the bromine-containing high-salt wastewater is metal smoke generated by calcining the smelting waste residue at high temperature, and is obtained by further recovering heavy metals from raffinate obtained by leaching, removing fluorine and chlorine, and extracting valuable metals.
S1.2, feeding the high-salinity wastewater subjected to secondary concentration into a one-effect evaporator to crystallize to obtain sodium chloride, centrifuging by using a centrifugal machine to obtain sodium chloride and sodium chloride mother liquor, and returning the sodium chloride mother liquor to the one-effect evaporator; sending the evaporation concentrated solution generated in the first-effect evaporator into a cooling crystallizer for crystallization to obtain potassium chloride, and separating the potassium chloride and mother liquor by a centrifugal machine; returning part of the mother liquor to the single-effect evaporator, taking part of the mother liquor as discharged mother liquor to perform bromine enrichment, and entering step S2 when the bromine in the discharged mother liquor is enriched to 2 g/L;
s2, distilling with water vapor to extract bromine, as shown in figure 2:
s2.1, pumping the discharged mother liquor subjected to bromine enrichment in the step S1.2 into a high-level tank, feeding the discharged mother liquor into a preheater by utilizing level difference, feeding the preheated discharged mother liquor into a distillation tower from the top of the distillation tower, carrying out an oxidation reaction of chlorine and a steam distillation process of free bromine in the distillation tower, and discharging the mother liquor from the bottom of the distillation tower after the reaction is finished; introducing water vapor from the bottom of the distillation tower, and introducing chlorine from the middle section of the distillation tower; the preheating temperature is 60-65 ℃;
s2.2, discharging bromine steam and part of water vapor distilled by the water vapor from the top of the distillation tower into a condenser, condensing the bromine steam and part of the water vapor into crude bromine (liquid bromine) and bromine water through heat exchange with cooling water in the condenser, and feeding the crude bromine (liquid bromine) and the bromine water into a bromine-water separation bottle; the uncondensed bromine vapor, water vapor and a small amount of chlorine gas enter an absorption tower, and exhaust gas is exhausted after absorption by discharged mother liquor;
s2.3, separating bromine and bromine water in a bromine water separation bottle by utilizing the difference of the gravities of the bromine and the bromine water, returning the bromine water to a distillation tower for redistillation, and rectifying crude bromine in a rectifying tower; after the crude bromine is rectified, free chlorine and other organic matters are greatly reduced, refined bromine discharged from the bottom of a rectifying tower enters a cooler for cooling, and then is put into a bromine storage bottle, and the finished bromine is obtained after the bromine storage bottle is packaged by a porcelain jar.
In this embodiment, the non-condensable gas may be used to preheat the bromine-containing high-salinity wastewater in step S1.1. Specifically, the bromine-containing high-salt wastewater is sent into a feeding tank, and heat exchange is carried out between a noncondensable gas heat exchanger and the bromine-containing high-salt wastewater.
In this embodiment, in step S2.3, the crude bromine is rectified twice by passing through the first-stage rectifying tower and the second-stage rectifying tower in sequence.
In this embodiment, in step S2.3, the tail gas generated in the rectifying tower enters the absorption tower, and the exhaust gas is exhausted after being absorbed by the discharged mother liquor.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (4)
1. A method for removing bromine from high-salinity wastewater is characterized by comprising the following steps:
s1, salt separation evaporation crystallization:
s1.1, preheating bromine-containing high-salinity wastewater, then sending the wastewater into a two-effect evaporator for primary concentration, and then sending the wastewater into a three-effect evaporator for secondary concentration; the preheating temperature is 80-85 ℃;
s1.2, feeding the high-salinity wastewater subjected to secondary concentration into a one-effect evaporator to crystallize to obtain sodium chloride, centrifuging by using a centrifugal machine to obtain sodium chloride and sodium chloride mother liquor, and returning the sodium chloride mother liquor to the one-effect evaporator; sending the evaporation concentrated solution generated in the first-effect evaporator into a cooling crystallizer for crystallization to obtain potassium chloride, and separating the potassium chloride and mother liquor by a centrifugal machine; returning part of the mother liquor to the single-effect evaporator, taking part of the mother liquor as discharged mother liquor to perform bromine enrichment, and entering step S2 when the bromine in the discharged mother liquor is enriched to 2 g/L;
s2, extracting bromine by steam distillation:
s2.1, pumping the discharged mother liquor subjected to bromine enrichment in the step S1.2 into a high-level tank, feeding the discharged mother liquor into a preheater by utilizing level difference, feeding the preheated discharged mother liquor into a distillation tower from the top of the distillation tower, carrying out an oxidation reaction of chlorine and a steam distillation process of free bromine in the distillation tower, and discharging the mother liquor from the bottom of the distillation tower after the reaction is finished; introducing water vapor from the bottom of the distillation tower, and introducing chlorine from the middle section of the distillation tower; the preheating temperature is 60-65 ℃;
s2.2, discharging bromine steam and part of water vapor distilled by the water vapor from the top of the distillation tower into a condenser, condensing the bromine steam and part of the water vapor into crude bromine and bromine water through heat exchange with cooling water in the condenser, and sending the crude bromine and the bromine water into a bromine-water separation bottle; the uncondensed bromine vapor, water vapor and a small amount of chlorine gas enter an absorption tower, and exhaust gas is exhausted after absorption by discharged mother liquor;
s2.3, separating bromine and bromine water in a bromine water separation bottle by utilizing the difference of the gravities of the bromine and the bromine water, returning the bromine water to a distillation tower for redistillation, and rectifying crude bromine in a rectifying tower; after the crude bromine is rectified, refined bromine discharged from the bottom of the rectifying tower enters a cooler for cooling, and then is put into a bromine storage bottle, and the finished bromine is obtained after the bromine storage bottle is packaged by a porcelain jar.
2. The method according to claim 1, characterized in that in step S1.1, the high-salinity wastewater containing bromine can be preheated by non-condensable gas.
3. The method according to claim 1, characterized in that in step S2.3, the crude bromine is subjected to twice rectification in sequence via a primary rectification column and a secondary rectification column.
4. The method according to claim 1, characterized in that in step S2.3, the tail gas generated in the rectifying tower enters an absorption tower, and the waste gas is exhausted after absorption by the discharged mother liquor.
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| CN202011482737.3A CN112707414A (en) | 2020-12-16 | 2020-12-16 | Method for removing bromine from high-salinity wastewater |
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| CN202011482737.3A CN112707414A (en) | 2020-12-16 | 2020-12-16 | Method for removing bromine from high-salinity wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115304083A (en) * | 2022-08-25 | 2022-11-08 | 湖北振华化学股份有限公司 | Method for circularly extracting bromine from glaserite mother liquor in production process of preparing potassium sulfate from glauber salt |
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