CN110548750B - Waste salt recycling treatment process and special equipment thereof - Google Patents
Waste salt recycling treatment process and special equipment thereof Download PDFInfo
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- CN110548750B CN110548750B CN201910836414.0A CN201910836414A CN110548750B CN 110548750 B CN110548750 B CN 110548750B CN 201910836414 A CN201910836414 A CN 201910836414A CN 110548750 B CN110548750 B CN 110548750B
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- sodium sulfate
- nanofiltration
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- 150000003839 salts Chemical class 0.000 title claims abstract description 149
- 239000002699 waste material Substances 0.000 title claims abstract description 51
- 238000004064 recycling Methods 0.000 title claims abstract description 33
- 238000011282 treatment Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 77
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 65
- 238000001728 nano-filtration Methods 0.000 claims abstract description 46
- 238000000926 separation method Methods 0.000 claims abstract description 43
- 239000012452 mother liquor Substances 0.000 claims abstract description 42
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 37
- 239000011780 sodium chloride Substances 0.000 claims abstract description 29
- 239000012535 impurity Substances 0.000 claims abstract description 26
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 26
- 238000001704 evaporation Methods 0.000 claims abstract description 25
- 230000008014 freezing Effects 0.000 claims abstract description 24
- 238000007710 freezing Methods 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 24
- 230000003647 oxidation Effects 0.000 claims abstract description 23
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 23
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 23
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 230000008020 evaporation Effects 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 10
- -1 sodium sulfate saturated brine Chemical class 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims description 16
- 230000008025 crystallization Effects 0.000 claims description 16
- 239000010413 mother solution Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000000701 coagulant Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000013589 supplement Substances 0.000 claims description 2
- 239000002920 hazardous waste Substances 0.000 description 6
- 238000010992 reflux Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/02—Gases or liquids enclosed in discarded articles, e.g. aerosol cans or cooling systems of refrigerators
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a waste salt recycling treatment process and special equipment thereof, wherein waste salt mainly comprising sodium chloride and sodium sulfate is respectively added with sodium chloride and sodium sulfate saturated brine to be continuously stirred, and filtered to obtain salt washing mother liquor, and precipitated sodium chloride and sodium sulfate solids are dried; freezing the salt-washing mother liquor, evaporating and crystallizing crystals, chemically removing impurities from the frozen mother liquor, removing organic and inorganic impurity ions, performing organic separation on impurity-removed effluent, utilizing in a mother liquor field, carrying out oxidation treatment on produced water, carrying out nanofiltration and salt separation on the oxidized produced water, returning nanofiltration concentrated water to a salt-washing system, and evaporating and drying nanofiltration produced water to obtain sodium chloride solid. According to the invention, through the effective combination of a series of processes such as salt washing, freezing, organic separation, oxidization, nanofiltration salt separation, evaporation and the like, sodium chloride and sodium sulfate in the waste salt are separated and purified, organic matters and other impurity ions in the waste salt are effectively separated or removed, the dangerous waste disposal cost is reduced, the recycling of the two waste salts is realized, and the economic value is created.
Description
Technical Field
The invention relates to the technical field of industrial waste salt treatment, in particular to a process and special equipment for separating and recycling industrial waste salt.
Background
In recent years, with the rapid development of economy in China, the amount of waste salt generated in the wastewater treatment process of industries such as domestic and foreign electric power petrochemical industry, coal chemical industry and the like also shows an increasing trend, and the annual yield of the waste salt exceeds 2000 ten thousand tons at present, and the waste salt is qualified as dangerous waste, so that strict control is required by the national environmental protection department. The waste salt which is not treated has the characteristic of easy leaching, can directly influence the pollution of surface water and underground water, and destroy the surrounding ecological environment, thereby leading to soil salinization and harm to the health of human bodies. Therefore, whether the waste salt can be properly treated and utilized becomes a key part of the zero-emission link of the wastewater.
The hazardous waste salt in the industries has the characteristics of mainly sodium chloride and sodium sulfate and containing a certain amount of organic matters, inorganic impurity ions such as calcium, magnesium, silicon and the like. At present, the hazardous waste salt treatment at home and abroad mainly adopts modes of incineration, landfill and the like. High temperature incineration refers to decomposing organic impurities in waste salt into gas under high temperature conditions, so that the content of organic matters in the waste salt is reduced to the standard required by industrial salt, but the waste salt cannot be obviously reduced simply by an incineration mode, and the equipment for high temperature decomposition also has the problems of ring formation, agglomeration and the like. Landfill disposal has the disadvantages of high cost and large occupied space, and industrial solid waste landfill sites are relatively few, so that hazardous waste salt is difficult to effectively dispose through landfill. Therefore, how to carry out resource treatment on the hazardous waste salt is a technical problem in the environmental protection industry and is a necessary requirement for environmental protection.
Chinese patent CN201611042295.4 discloses a method for recycling the mixed salt produced by industrial wastewater treatment. The mixed salt generated in the industrial wastewater treatment process is subjected to treatment means such as calcination, solid-liquid separation, evaporative crystallization and the like, but the temperature during calcination is too high, and the whole system has the defects of higher energy consumption, difficult control and the like.
Chinese patent CN201720193387.6 discloses a chemical industry waste water solid waste salt resourceful treatment system, which is characterized in that solid waste salt prepared by evaporating and crystallizing high-concentration brine in the coal chemical industry is reacted with sulfuric acid in the modes of mixing reaction, storage, hydrogen chloride absorption, washing centrifugal treatment, hot air drying, packaging and the like to produce hydrogen chloride and sodium bisulfate crystals, and the sulfuric acid is added, so that a certain medicament cost is increased, and organic species in some waste salt in the coal chemical industry are complex, high in content and poor in removal effect, so that the real purification and resourceful treatment cannot be realized.
Disclosure of Invention
Aiming at the problems of complex treatment process, difficult separation of organic matters, high operation energy consumption and high implementation cost of the existing hazardous waste salt treatment process, the invention provides a waste salt recycling treatment process and special equipment thereof, and the sodium chloride and sodium sulfate in the waste salt are separated and purified through the effective combination of a series of processes of salt washing, freezing, organic separation, oxidization, nanofiltration salt separation, evaporation and the like, so that the process is clear and controllable, the organic matters and other impurity ions in the waste salt are effectively separated or removed, the pollution of the waste salt to the surrounding environment is effectively reduced, the hazardous waste treatment cost is reduced, the recycling of the two waste salts is realized, and the economic value is created.
Technical proposal
In order to achieve the technical aim, the invention provides a waste salt recycling treatment process which is characterized by comprising the following steps:
(1) Washing salt: adding sodium chloride saturated brine into waste salt mainly comprising sodium chloride, continuously stirring, filtering to obtain salt washing mother liquor I, drying precipitated sodium chloride solid, and recycling condensed water;
washing salt with waste salt mainly comprising sodium sulfate to obtain a salt washing mother solution II, or continuously stirring with saturated sodium sulfate salt water, filtering to obtain a salt washing mother solution III, drying precipitated sodium sulfate solid, and recycling condensed water;
(2) Freezing and crystallizing: mixing the salt washing mother liquor I and the salt washing mother liquor II or the salt washing mother liquor I and the salt washing mother liquor III obtained in the step (1), and performing freezing treatment on the mixed salt washing mother liquor to obtain sodium sulfate decahydrate crystals and frozen mother liquor, and performing evaporation crystallization on the sodium sulfate decahydrate crystals to obtain anhydrous sodium sulfate;
(3) Chemical impurity removal: carrying out chemical impurity removal on the frozen mother liquor obtained in the step (2) to remove calcium and magnesium, heavy metals, organic and inorganic impurity ions and obtain supernatant and precipitate;
(4) Organic separation: continuing to carry out organic separation on the supernatant obtained in the step (3), and carrying out separation treatment on organic matters and salts to obtain organic separation produced water and organic separation mother liquor, wherein the mother liquor is utilized in a field;
(5) Oxidizing: oxidizing the organic matters in the organic separation produced water obtained in the step (4) to obtain oxidized produced water;
(6) Nanofiltration and salt separation: carrying out nanofiltration salt separation treatment on the oxidized produced water obtained in the step (5) to obtain nanofiltration concentrated water and nanofiltration produced water, returning the nanofiltration concentrated water to a salt washing system, concentrating, evaporating and drying the nanofiltration produced water to obtain sodium chloride solid, and recycling condensed water;
Further, in the step (1), sodium chloride is mainly waste salt, and when precipitated sodium chloride solid is filtered, the solid is dried at the temperature of 60-80 ℃;
Salt is washed by waste salt mainly containing sodium sulfate, the salt washing temperature is controlled to be 20-60 ℃, the rotating speed is controlled to be 20-100r/min, a salt washing mother solution II is obtained, or saturated brine of sodium sulfate is added to be 20-60 ℃, the rotating speed is controlled to be 20-100r/min, the reaction time is continuously stirred for 20-90min, precipitated sodium sulfate solid is dried at 60-80 ℃, condensed water is recycled, and a salt washing mother solution III is obtained through filtration.
Further, freezing the salt-washing mother liquor in the step (2) at the temperature of-10 ℃ to obtain sodium sulfate decahydrate crystals, and then evaporating and crystallizing to obtain anhydrous sodium sulfate;
Further, adding alkali into the frozen mother solution obtained in the step (3) to adjust the pH to 9-12, adding a coagulant, a heavy supplement and the like to remove organic and inorganic impurity ions such as calcium, magnesium, heavy metals and the like, and obtaining supernatant and precipitate;
Further, the supernatant fluid obtained in the step (4) enters an organic separation system, the operation pressure is 5-40bar, the pH value is 5-9, organic matters and salt are separated, and the organic separated mother liquor is utilized in a field;
Further, the produced water obtained by organic concentration and separation in the step (5) enters an oxidation system, the pH is between 8 and 11 by utilizing an advanced oxidation mode (such as Fenton oxidation, ozone catalytic oxidation and the like), the oxidation time is 30 to 90 minutes, and the oxidized produced water enters a nanofiltration system;
And (3) feeding the oxidized water produced in the step (6) into a nanofiltration system, wherein the operating pressure is 10-60bar, the nanofiltration concentrated water returns to the salt-washing mother liquor, the nanofiltration water produced is concentrated, evaporated and crystallized to obtain sodium chloride solid, and the condensate water is recycled.
The special equipment for the waste salt recycling treatment process is characterized in that: the device comprises a salt washing system A, a salt washing system B, a dryer A, a dryer B, a freezing and crystallizing system, a impurity removing system, an organic separation system, an oxidation reactor, a nanofiltration system, an evaporation and crystallizing system, a sodium chloride salt collecting system A, a sodium chloride salt collecting system B, a sodium sulfate salt collecting system A, a sodium sulfate salt collecting system B, a first water inlet pump and a second water inlet pump;
The liquid output end of the salt washing system A and the discharge port of the salt washing system B are connected with the feed port of the freezing and crystallizing system, the solid output end of the salt washing system A is connected with the sodium chloride salt collecting system A, and the solid output end of the salt washing system B is connected with the sodium sulfate salt collecting system B; the crystal output end of the freezing crystallization system is connected with a sodium sulfate salt collecting system A, and the mother liquor output end of the freezing crystallization system is connected with the inlet of the impurity removal system; the outlet of the impurity removal system is connected with the organic separation system, and a first water inlet pump is arranged on the connecting pipeline; the water output end of the organic separation system is connected with the oxidation reactor; the outlet of the oxidation reactor is connected with a nanofiltration system, a second water inlet pump is arranged on a connecting pipeline, the concentrated water output end of the nanofiltration system is connected with the reflux port of the salt washing system B, the produced water output end of the nanofiltration system is connected with an evaporation crystallization system, the crystal output end of the evaporation crystallization system is connected with a sodium chloride salt collecting system B, and the condensate output end of the evaporation crystallization system is connected for recycling.
Further, the salt washing system A is provided with a first feeding end for allowing saturated brine of sodium chloride to enter the salt washing system;
further, the salt washing system B is provided with a feeding end II for sodium sulfate saturated brine to enter the salt washing system, and a reflux end for concentrated water of the nanofiltration system to reflux into the salt washing system.
Advantageous effects
The invention provides a waste salt recycling treatment process and special equipment, which separate and purify sodium chloride and sodium sulfate in waste salt through a series of effective combination of salt washing, freezing, organic separation, oxidization, nanofiltration salt separation, evaporation and other processes, has clear and controllable process, effectively separates or removes organic matters and other impurity ions in the waste salt, can effectively reduce pollution of the waste salt to the surrounding environment, reduces dangerous waste disposal cost, realizes recycling of the two waste salts and creates economic value.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present invention.
Fig. 2 is a schematic diagram of a connection relationship of dedicated devices in an embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Examples
As shown in figure 2, the special equipment for the waste salt recycling treatment process comprises a salt washing system A1, a salt washing system B2, a dryer A3, a dryer B3', a freezing and crystallizing system 4, a impurity removing system 5, an organic separation system 6, an oxidation reactor 7, a nanofiltration system 8, an evaporation and crystallizing system 9, a sodium chloride salt collecting system A10, a sodium chloride salt collecting system B11, a sodium sulfate salt collecting system A12, a sodium sulfate salt collecting system B10', a first water inlet pump 13 and a second water inlet pump 14;
The liquid output end of the salt washing system A1 and the discharge port c 'of the salt washing system B2 are connected with the feed port of the freezing and crystallizing system 4, the solid output end of the salt washing system A1 is connected with the sodium chloride salt collecting system A10, and the solid output end of the salt washing system B2 is connected with the sodium sulfate salt collecting system B10'; the crystal output end of the freezing and crystallizing system 4 is connected with a sodium sulfate salt collecting system A12, and the mother liquor output end of the freezing and crystallizing system 4 is connected with the inlet of the impurity removing system 5; the outlet of the impurity removal system 5 is connected with the organic separation system 6, and a first water inlet pump 13 is arranged on the connecting pipeline; the water output end of the organic separation system 6 is connected with the oxidation reactor 7; the outlet of the oxidation reactor 7 is connected with a nanofiltration system 8, a second water inlet pump 14 is arranged on a connecting pipeline, the concentrated water output end of the nanofiltration system 8 is connected with the reflux end B' of the salt washing system B2, the produced water output end of the nanofiltration system 8 is connected with an evaporation crystallization system 9, the crystal output end of the evaporation crystallization system 9 is connected with a sodium chloride salt collecting system B11, and the condensate output end of the evaporation crystallization system 9 is connected for recycling.
The salt washing system A1 is provided with a feeding end a for sodium chloride saturated brine to enter the salt washing system;
the salt washing system B2 is provided with a feeding end a 'for sodium sulfate saturated brine to enter the salt washing system, and the salt washing system B2 is provided with a reflux end B' for concentrated water of the nanofiltration system 8 to reflux into the salt washing system;
As shown in figure 1, the waste salt recycling treatment process by using the special equipment comprises the following steps:
Firstly, adding sodium chloride saturated brine into waste salt mainly containing sodium chloride, controlling the temperature at 20-60 ℃, controlling the rotating speed at 20-100r/min, continuously stirring for 20-90min, drying precipitated sodium chloride solids at 60-80 ℃, recycling condensed water, filtering to obtain salt-washing mother liquor I, washing salt with waste salt mainly containing sodium sulfate, controlling the temperature at 20-60 ℃ and the rotating speed at 20-100r/min to obtain salt-washing mother liquor II, or adding sodium sulfate saturated brine at 20-60 ℃, controlling the rotating speed at 20-100r/min, continuously stirring for 20-90min, drying precipitated sodium sulfate solids at 60-80 ℃, recycling condensed water, and filtering to obtain salt-washing mother liquor III;
Freezing the mixed salt washing mother liquor obtained in the first step at the temperature of minus 10-10 ℃ to obtain sodium sulfate decahydrate crystals, then evaporating and crystallizing to obtain anhydrous sodium sulfate, and enabling the frozen mother liquor to enter the next step;
Thirdly, regulating the pH value of the frozen mother liquor obtained in the second step to 9-12, adding a coagulant, a heavy-duty agent and the like to remove organic and inorganic impurity ions such as calcium, magnesium, heavy metals and the like, and obtaining supernatant and precipitate;
fourthly, continuing to carry out organic separation on the supernatant obtained in the third step, separating and treating organic matters and salt at the operating pressure of 5-40bar and the pH value of 5-9, utilizing the organic separated mother liquor in a field, and enabling the organic separated produced water to enter the next step;
Fifthly, adding an oxidant (such as ozone, hydrogen peroxide and the like) into the produced water obtained by the organic concentration and separation in the fourth step, oxidizing the organic matters in the produced water, utilizing a high-grade oxidation mode (such as Fenton oxidation, ozone catalytic oxidation and the like), enabling the pH to be between 8 and 11, enabling the oxidation time to be 30-90min, and enabling the oxidized produced water to enter a nanofiltration system;
And sixthly, carrying out nanofiltration and salt separation on the oxidized water produced in the fifth step, wherein the operating pressure is 10-60ar, so as to obtain nanofiltration water produced and nanofiltration concentrated water, returning the nanofiltration concentrated water to the salt washing mother liquor, concentrating, evaporating and drying the nanofiltration water produced, so as to obtain sodium chloride solid, and recycling condensed water.
Claims (8)
1. The waste salt recycling treatment process is characterized by comprising the following steps of:
(1) Washing salt: adding sodium chloride saturated brine into waste salt mainly comprising sodium chloride, continuously stirring, filtering to obtain salt washing mother liquor I, drying precipitated sodium chloride solid, and recycling condensed water;
washing salt with waste salt mainly comprising sodium sulfate to obtain a salt washing mother solution II, or continuously stirring with saturated sodium sulfate salt water, filtering to obtain a salt washing mother solution III, drying precipitated sodium sulfate solid, and recycling condensed water;
(2) Freezing and crystallizing: mixing the salt washing mother liquor I and the salt washing mother liquor II or the salt washing mother liquor I and the salt washing mother liquor III obtained in the step (1), and performing freezing treatment on the mixed salt washing mother liquor to obtain sodium sulfate decahydrate crystals and frozen mother liquor, and performing evaporation crystallization on the sodium sulfate decahydrate crystals to obtain anhydrous sodium sulfate;
(3) Chemical impurity removal: carrying out chemical impurity removal on the frozen mother liquor obtained in the step (2) to remove calcium and magnesium, heavy metals, organic and inorganic impurity ions and obtain supernatant and precipitate;
(4) Organic separation: continuing to carry out organic separation on the supernatant obtained in the step (3), and carrying out separation treatment on organic matters and salts to obtain organic separation produced water and organic separation mother liquor, wherein the mother liquor is utilized in a field;
(5) Oxidizing: oxidizing the organic matters in the organic separation produced water obtained in the step (4) to obtain oxidized produced water;
(6) Nanofiltration and salt separation: and (3) carrying out nanofiltration salt separation treatment on the oxidized produced water obtained in the step (5) to obtain nanofiltration concentrated water and nanofiltration produced water, returning the nanofiltration concentrated water to a salt washing system, concentrating, evaporating and drying the nanofiltration produced water to obtain sodium chloride solid, and recycling condensed water.
2. The process for recycling waste salt according to claim 1, which is characterized in that:
The waste salt mainly containing sodium chloride in the step (1) is dried at the temperature of 60-80 ℃ when the precipitated sodium chloride solid is filtered;
Salt is washed by waste salt mainly containing sodium sulfate, the salt washing temperature is controlled to be 20-60 ℃, the rotating speed is controlled to be 20-100r/min, a salt washing mother solution II is obtained, or saturated brine of sodium sulfate is added to be 20-60 ℃, the rotating speed is controlled to be 20-100r/min, the reaction time is continuously stirred for 20-90min, precipitated sodium sulfate solid is dried at 60-80 ℃, condensed water is recycled, and a salt washing mother solution III is obtained through filtration.
3. The process for recycling waste salt according to claim 1, which is characterized in that: and (3) freezing the salt-washing mother liquor mixed in the step (2) at the temperature of between 10 ℃ below zero and 10 ℃ to obtain sodium sulfate decahydrate crystals, and then evaporating and crystallizing to obtain anhydrous sodium sulfate.
4. The process for recycling waste salt according to claim 1, which is characterized in that: adding alkali into the frozen mother solution obtained in the step (3) to adjust the pH value to 9-12, adding a coagulant and a heavy supplement to remove calcium and magnesium, heavy metals and organic and inorganic impurity ions, and obtaining supernatant and precipitate.
5. The process for recycling waste salt according to claim 1, which is characterized in that: and (3) performing organic separation treatment on the supernatant in the step (4), wherein the operating pressure is 5-40bar, the pH value is 5-9, separating organic matters from salt, and utilizing the organic matters and salt in an organic separated mother liquor field.
6. The process for recycling waste salt according to claim 1, which is characterized in that: and (3) carrying out Fenton oxidation or ozone catalytic oxidation treatment on the organic separation produced water in the step (5), wherein the pH value is 8-11, the oxidation time is 30-90min, and the obtained oxidized produced water is subjected to nanofiltration treatment.
7. The process for recycling waste salt according to claim 1, which is characterized in that: when the oxidation water produced in the step (6) is subjected to nanofiltration treatment, the nanofiltration concentrated water returns to the salt-washing mother liquor under the operating pressure of 10-60bar, the nanofiltration water produced is concentrated, evaporated and crystallized to obtain sodium chloride solid, and the condensed water is recycled.
8. A special device for a waste salt recycling process according to any one of the preceding claims, characterized in that: the system comprises a salt washing system A (1), a salt washing system B (2), a dryer A (3), a dryer B (3 '), a freezing and crystallizing system (4), a impurity removing system (5), an organic separation system (6), an oxidation reactor (7), a nanofiltration system (8), an evaporation and crystallizing system (9), a sodium chloride salt collecting system A (10), a sodium chloride salt collecting system B (11), a sodium sulfate salt collecting system A (12), a sodium sulfate salt collecting system B (10'), a first water inlet pump (13) and a second water inlet pump (14);
The liquid output end of the salt washing system A (1) and the discharge port (c ') of the salt washing system B (2) are respectively connected with the feed port of the freezing crystallization system (4), the solid output end of the salt washing system A (1) is connected with the sodium chloride salt collecting system A (10), the solid output end of the salt washing system B (2) is connected with the sodium sulfate salt collecting system B (10 '), the crystal output end of the freezing crystallization system (4) is connected with the sodium sulfate salt collecting system A (12), the mother liquor output end of the freezing crystallization system (4) is connected with the inlet of the impurity removing system (5), the outlet of the impurity removing system (5) is connected with the organic separation system (6), the impurity removing system (5) is provided with a first water inlet pump (13) on the connecting pipe of the organic separation system (6), the water producing output end of the organic separation system (6) is connected with the oxidation reactor (7), the outlet of the oxidation reactor (7) is connected with the nanofiltration system (8), the second water inlet pump (14) is arranged on the path of the nanofiltration system (8), the mother liquor output end of the freezing crystallization system (4) is connected with the crystal output end of the evaporation system (9 ') of the evaporation system (9) which is connected with the crystal output end of the crystal (9), the condensate output end of the evaporative crystallization system (9) is connected and reused;
The salt washing system A (1) is provided with a first feeding end (a) for allowing saturated brine of sodium chloride to enter the salt washing system;
The salt washing system B (2) is provided with a feeding end II (a ') for sodium sulfate saturated brine to enter the salt washing system, and the salt washing system B (2) is provided with a backflow end (B') for concentrated water of the nanofiltration system (8) to flow back into the salt washing system.
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| CN113772692A (en) * | 2021-09-03 | 2021-12-10 | 江苏海普功能材料有限公司 | Method for treating and recycling waste salt |
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