CN116161756A - Preparation method of heavy medium for treating wastewater containing multiple pollutants - Google Patents
Preparation method of heavy medium for treating wastewater containing multiple pollutants Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 33
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000002223 garnet Substances 0.000 claims abstract description 12
- 239000011550 stock solution Substances 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000002023 wood Substances 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 5
- AVXURJPOCDRRFD-UHFFFAOYSA-N hydroxylamine group Chemical group NO AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 239000011591 potassium Substances 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
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- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 5
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 230000004048 modification Effects 0.000 claims abstract description 3
- 238000012986 modification Methods 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
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- 238000011282 treatment Methods 0.000 claims description 18
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- 238000001764 infiltration Methods 0.000 claims description 10
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
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- 230000002378 acidificating effect Effects 0.000 claims description 5
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
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- 230000001360 synchronised effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- 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
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- 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
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- 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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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a preparation method of a heavy medium for treating wastewater containing multiple pollutants, which comprises the steps of firstly treating acid mine wastewater with colored residues, and carrying out sulfuric acid washing to obtain a stock solution containing Fe, al and Mn metal ions, wherein the acid mine wastewater with colored residues is treated with the acid mine wastewater with colored residues: garnet: sawing wood powder: the mass ratio of the gelatinizer is 3-6: 1-2: 1-2: 1, a step of; regulating the pH value of the stock solution, stirring and infiltrating to obtain an infiltrating solution, adding a reducing agent with the ratio of 0.02-0.2 kg/L to the infiltrating solution for modification, wherein the reducing agent is hydroxylamine, sodium borohydride or potassium borohydride, filtering to obtain a filter cake, granulating the precursor, and drying, roasting and cooling to obtain the heavy medium for treating wastewater containing multiple pollutants. The heavy medium obtained by the invention has multiple groups, multiple pores, high specific surface area and high specific gravity, and has good wastewater treatment effect on COD, cu, pb, zn, cd, as and other pollutants, good index and good sedimentation performance.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a preparation method of a heavy medium for wastewater treatment containing multiple pollutants, in particular to a method for preparing the heavy medium by taking acid wastewater treatment bottom slag of a colored mine as a main raw material.
Background
Along with the sustainable development of social economy in China, the industrial industry is rapidly expanded, the industrial wastewater is continuously increased in the production process of industrial enterprises, the industrial wastewater generally has the characteristics of multiple pollutant types, high concentration and the like, and particularly in the industries of electronics, electroplating, mineral processing, metallurgy and the like, the industrial wastewater contains pollutants such as COD, multiple heavy metals, fluorine and the like, and the treatment difficulty is high. For COD-containing wastewater, a chemical oxidation method is a common and most effective treatment mode, and a chemical agent with oxidizing property is required to be used, and a catalyst is required to be matched for use; for wastewater containing heavy metals, a lime neutralization method is generally adopted, and pollutants are made to generate indissolvable metal hydroxides by increasing the pH value of the wastewater, but different heavy metals have different precipitation pH values, so that the process is difficult to control. For wastewater containing various pollutants, a sectional treatment mode is adopted according to the characteristics of different pollutants, and the same treatment method and process are difficult to synchronously treat the various pollutants, so that the wastewater treatment difficulty is high, the process is complex, and the facility equipment requirement is high.
In the treatment process of various pollutants, pollutant ions are generally reacted with other substances to generate indissolvable compounds, and then the pollutants are removed from the wastewater through flocculation reaction and solid-liquid separation. The generated compound exists in the form of molecules in the wastewater, and has extremely fine granularity. Even through flocculation of the flocculant, the generated floccule particles have the problems of small particle size, low specific gravity and high water content, so that the floccule particles have low sedimentation speed, the content of effluent SS is high, and the concentration of effluent detection pollutants is further increased. The design can only slow down the problem by increasing the type selection of the sedimentation equipment, and the problem of large occupied area of treatment facilities and high investment cost can be brought.
Therefore, the development of the water treatment product which is suitable for synchronous treatment of various pollutants, has excellent effect and good sedimentation effect has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of a heavy medium for treating wastewater containing multiple pollutants.
The invention comprises the following steps:
a) Treating the bottom slag of the acid waste water of the colored mine, and carrying out sulfuric acid washing to obtain a stock solution containing various metal ions such as Fe, al, mn and the like; the sulfuric acid concentration is 10 of hydrogen ion content -2 ～10 -3 mol/L, the dosage is 3-6L sulfuric acid: 1 kg acid mine waste water treatment bottom slag.
b) Adding garnet, saw dust and a gelatinizing agent into the stock solution obtained in the step a), and infiltrating in the stirring process to obtain an infiltration solution; acid mine waste water treatment bottom slag: garnet: sawing wood powder: the mass ratio of the gelatinizer is 3-6: 1-2: 1-2: 1.
c) Regulating the pH value of the infiltration liquid obtained in the step b) by adopting caustic soda flakes, adding a reducing agent, modifying in the combined process of stirring and ultrasonic treatment, and taking a filtered filter cake as a precursor; the reducing agent is one of hydroxylamine, sodium borohydride and potassium borohydride, and the dosage is 0.02-0.2 kg/L of infiltration liquid.
d) Granulating the precursor obtained in the step c), drying in a protective gas, roasting, and cooling to obtain the heavy medium.
The colored mine acidic wastewater treatment bottom slag in the step a) contains 8-12% of iron, 2-8% of aluminum, 1-4% of manganese and 8-15% of calcium.
And a) treating the bottom slag by using acid waste water of the colored mine, wherein the residual insoluble matters after acid washing are gypsum.
The soaking time in the step b) is controlled to be 60-180 min.
The pH in step c) is controlled between 6 and 8.
The stirring speed in the step c) is 1000-2000 r/min, the power of ultrasound is 100-120W, the working frequency is 25-40 KHz, and the modification treatment time is controlled to be 30-60 min.
The precursor obtained in the step c) is solid particles with a large number of active groups such as hydroxyl, sulfhydryl, carboxyl and the like and reducing metal elements.
The particle size of the granules in step d) is 0.038 to 1.5. 1.5 mm.
The shielding gas in the step d) is one of hydrogen and nitrogen.
The roasting temperature in the step d) is 500-1200 ℃ and the roasting time is 30-120 min.
The invention uses the acid mine wastewater treatment bottom slag as the raw material, solves the problem of solid wastewater stockpiling and disposal of enterprises, and reduces environmental protection risks; the invention prepares the bottom slag which originally belongs to the solid waste category into the product, and simultaneously produces the gypsum product, thereby bringing double economic benefits for enterprises.
The invention utilizes the various characteristics of adsorption, catalysis and the like of various metal ions existing in the colored mine acidic wastewater treatment bottom slag, and adjusts the morphology and occurrence state of the metal ions through the processes of infiltration, reduction and burning; meanwhile, in the process of preparing the precursor by using the wetting liquid, hydroxylamine, sodium borohydride or potassium borohydride serving as reducing agents are selected and mixed with the wetting liquid according to the proportion of 0.02-0.2 kg/L, so that a large amount of active groups such as hydroxyl groups, mercapto groups and carboxyl groups and reducing metal elements are attached to solid particles of the precursor, and the active groups and the reducing metal elements are dehydrated, solidified and attached in a porous structure in the roasting process of the reducing atmosphere. Finally forming a heavy medium with multiple groups, multiple pores, high specific surface area and high specific gravity, and activating the solidified active groups after absorbing water in wastewater treatment, wherein the activated groups in the porous structure have adsorption and condensation effects on COD, heavy metals and the like; the reducing metal element has catalytic effect on COD, mn and other treatments; under the characteristic of high specific gravity of the heavy medium, each pollutant is accelerated to subside along with the heavy medium, and the solid-liquid separation effect is excellent. Under the multiple actions of adsorption, condensation and catalysis, the method has high-efficiency treatment effect on wastewater containing COD, heavy metals, mn, SS and other multi-pollutants.
Drawings
FIG. 1 is an electron micrograph of a heavy medium for water treatment prepared in example 1 of the present invention; (a) 500 x image of the product obtained in example 1 and (b) 5000 x image of the product obtained in example 1.
FIG. 2 shows the multi-pollutant removal rate of hydrometallurgical wastewater of the heavy medium for water treatment prepared in example 1 of the present invention.
FIG. 3 shows the sedimentation velocity and effluent SS of the product obtained in example 1 of the present invention compared with those of a conventional beneficiation wastewater treatment process for a hydrometallurgical wastewater treatment; wherein (a) is the sedimentation velocity; (b) is effluent SS.
FIG. 4 shows the multi-pollutant removal rate of alkaline wash wastewater from a certain smelter of the heavy media for water treatment prepared in example 2 of the present invention.
FIG. 5 shows the effect of the product of example 2 of the present invention compared with the sedimentation velocity and effluent SS of a conventional treatment process for alkaline wash wastewater treatment in a certain smeltery; wherein (a) is the sedimentation velocity; (b) is effluent SS.
Fig. 6 is a flow chart of the present invention.
Detailed Description
The following is a specific embodiment of the present invention, and the technical solution of the present invention is further described, but the present invention is not limited to this embodiment.
Example 1
The flow of the present invention is shown in fig. 6.
The preparation method of the heavy medium for treating wastewater containing multiple pollutants comprises the following specific steps:
a) The acid waste water treatment bottom slag of the colored mine contains 11.2 percent of iron, 3.4 percent of aluminum, 3.2 percent of manganese, 12.1 percent of calcium and 10 percent of hydrogen ions -2 And (3) carrying out acid washing on the acid waste water treatment bottom slag of the 1 kg colored mine by using the sulfuric acid 5L with mol/L to obtain a stock solution.
b) Treating the bottom slag according to the acid mine wastewater: garnet: sawing wood powder: gellant mass ratio 4:1.6:1.4:1, adding garnet, saw dust and a gelatinizing agent into the stock solution, stirring and soaking for 150 min.
c) Adjusting the pH value of the infiltration liquid to 7 by adopting caustic soda flakes, adding sodium borohydride according to the dosage of 0.15 kg/L, modifying in the combined process of stirring rotation speed of 1200 r/min, ultrasonic power of 120W and ultrasonic frequency of 25 KHz, filtering after modifying for 60 min, and taking the filter cake as a precursor.
d) Granulating the precursor, wherein the particle size of the granules is 0.045-1.5 and mm, drying, roasting and cooling in the presence of hydrogen, and roasting at 650 ℃ for 45 min to obtain the heavy medium.
The specific surface area of the product obtained in example 1 of the present invention was 313 and 313 m 2 /g。
An electron microscope photograph of the product obtained in example 1 of the present invention is shown in fig. 1.
The product obtained in example 1 of the present invention is shown in fig. 2 compared with the pollutant removal effect of a conventional beneficiation wastewater treatment process on a certain hydrometallurgical wastewater treatment.
The sedimentation effect of the product obtained in the embodiment 1 of the invention on a hydrometallurgical wastewater treatment is compared with that of a conventional beneficiation wastewater treatment process, and is shown in fig. 3.
Example 2
The preparation method of the heavy medium for treating wastewater containing multiple pollutants comprises the following specific steps:
a) The acid waste water treatment bottom slag of the colored mine contains 9.2 percent of iron, 7.8 percent of aluminum, 2.1 percent of manganese, 9.6 percent of calcium and 10 percent of hydrogen ions -3 And (3) carrying out acid washing on the acid waste water treatment bottom slag of the 1 kg colored mine by using the sulfuric acid 4L with mol/L to obtain a stock solution.
b) Treating the bottom slag according to the acid mine wastewater: garnet: sawing wood powder: gellant mass ratio 6:1:1:1, adding garnet, saw dust and a gelatinizing agent into the stock solution, stirring and soaking for 90 min.
c) Adjusting the pH value of the infiltration liquid to 6.5 by adopting caustic soda flakes, adding hydroxylamine according to the dosage of 0.05 kg/L, modifying in the combined process of stirring rotation speed of 1200 r/min, ultrasonic power of 100W and ultrasonic frequency of 30 KHz, filtering after modifying for 30 min, and taking the filter cake as a precursor.
d) Granulating the precursor, wherein the particle size of the granules is 0.038-0.074 and mm, drying, roasting and cooling in the protection of nitrogen, and roasting at 1150 ℃ for 120 min to obtain the heavy medium.
The product obtained in example 2 of the present invention has a specific surface area of 263 m 2 /g。
The product obtained in the embodiment 2 of the invention is compared with the conventional treatment method to remove multiple pollutants from alkaline washing wastewater of a certain smelting plant, and the effect is shown in fig. 4.
The sedimentation effect of the product obtained in the embodiment 2 of the invention on the alkali wash wastewater treatment of a certain smelting plant is compared with that of the conventional treatment method, and is shown in figure 5.
Example 3
The preparation method of the heavy medium for treating wastewater containing multiple pollutants comprises the following specific steps:
a) The acid waste water treatment bottom slag of the colored mine contains 10.4 percent of iron, 6.3 percent of aluminum, 1.4 percent of manganese, 14.3 percent of calcium and 10 percent of hydrogen ions -2 mol/L sulfuric acid 6L for treating 1 kg colored mine acidic wastewaterAnd (5) pickling the bottom slag to obtain a stock solution.
b) Treating the bottom slag according to the acid mine wastewater: garnet: sawing wood powder: gellant mass ratio 4:1:2:1, adding garnet, saw dust and a gelatinizing agent into the stock solution, stirring and soaking for 90 min.
c) Adopting caustic soda flakes to adjust the pH value of the infiltration liquid to 7.0, adding potassium borohydride according to the dosage of 0.1 kg/L, modifying in the combined process of stirring rotation speed of 1200 r/min, ultrasonic power of 120W and ultrasonic frequency of 30 KHz, filtering after modifying for 45 min, and taking the filter cake as a precursor.
d) Granulating the precursor, wherein the particle size of the granules is 0.074-0.125 mm, drying, roasting and cooling in the protection of nitrogen, and roasting at 800 ℃ for 90 min to obtain the heavy medium.
The specific surface area of the product obtained in example 3 of the present invention was 383 m 2 /g。
Claims (7)
1. The preparation method of the heavy medium for treating the wastewater containing multiple pollutants is characterized by comprising the following steps:
a) Treating the bottom slag with acid waste water of the nonferrous mine, and carrying out sulfuric acid washing to obtain a stock solution containing Fe, al and Mn metal ions;
b) Adding garnet, saw dust and a gelatinizing agent into the stock solution obtained in the step a), wherein the quality of the colored mine acidic wastewater treatment bottom slag, the garnet, the saw dust and the gelatinizing agent is as follows: garnet: sawing wood powder: gellant = 3-6: 1-2: 1-2: 1, a step of; infiltrating in the stirring process to obtain an infiltration liquid; the sulfuric acid concentration is 10 of hydrogen ion content -2 ～10 -3 mol/L, the dosage is 3-6L sulfuric acid: 1 kg treating the acid mine waste water with bottom slag;
c) Regulating the pH value of the infiltration liquid obtained in the step b) by adopting caustic soda flakes, adding a reducing agent, modifying in the combined process of stirring and ultrasonic treatment, wherein a filtered filter cake is a precursor, and a large amount of hydroxyl, sulfhydryl and carboxyl active groups and reducing metal elements are attached to solid particles of the precursor; the reducing agent is hydroxylamine, sodium borohydride or potassium borohydride, and the ratio of the reducing agent to the infiltration liquid is 0.02-0.2 kg/L;
d) And c) granulating the precursor obtained in the step c), and then placing the granulated precursor in a protective gas for drying, roasting and cooling to obtain the heavy medium for treating wastewater containing multiple pollutants.
2. The method for preparing the heavy medium for treating wastewater containing multiple pollutants according to claim 1, wherein in the step a), the mass content of iron in the acidic wastewater treatment bottom slag of the colored mine is 8-12%, the mass content of aluminum is 2-8%, the mass content of manganese is 1-4%, and the mass content of calcium is 8-15%.
3. The method for preparing a heavy medium for treating wastewater containing multiple pollutants according to claim 1, wherein the soaking time in the step b) is 60-180 min.
4. The method for producing a heavy medium for wastewater treatment containing multiple pollutants according to claim 1, wherein the pH in step c) is controlled to be 6 to 8.
5. The method for preparing a heavy medium for wastewater treatment containing multiple pollutants according to claim 1, wherein the stirring speed in the step c) is 1000-2000 r/min, the ultrasonic power is 100-120W, the working frequency is 25-40 KHz, and the modification treatment time is controlled to be 30-60 min.
6. The method for producing a heavy medium for wastewater treatment containing multiple pollutants according to claim 1, wherein the particle size of the granules in the step d) is 0.038 to 1.5. 1.5 mm.
7. The method for preparing a heavy medium for wastewater treatment containing multiple pollutants according to claim 1, wherein the shielding gas in the step d) is one of hydrogen and nitrogen; the roasting temperature is 500-1200 ℃ and the roasting time is 30-120 min.
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