CN113479989B - Pretreatment method for coal gas water seal water pipeline - Google Patents
Pretreatment method for coal gas water seal water pipeline Download PDFInfo
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- CN113479989B CN113479989B CN202110798750.8A CN202110798750A CN113479989B CN 113479989 B CN113479989 B CN 113479989B CN 202110798750 A CN202110798750 A CN 202110798750A CN 113479989 B CN113479989 B CN 113479989B
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/78—Details relating to ozone treatment devices
- C02F2201/784—Diffusers or nozzles for ozonation
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
Abstract
The invention discloses a pretreatment method of a coal gas water seal pipeline, which belongs to the technical field of wastewater treatment, and the method comprises the following steps of: (1) Adding an active carbon catalyst loaded with nano manganese ferrite, a persulfate oxidant and micro-nano bubble ozone into water, mixing and reacting for 15-40 min through a pipeline static mixer, so that the molecular structure of toxic substances in the wastewater is destroyed, and the biotoxicity of the toxic substances is reduced; (2) After the reaction is finished, a magnetic device is used for recycling the catalyst, the demagnetizer is used for demagnetizing the recycled catalyst, deionized water and absolute ethyl alcohol are respectively used for washing 5-8 times, and the catalyst is returned for reuse; (3) After pretreatment, BOD/COD of the wastewater rises to above 0.25, and the wastewater can directly enter a coking wastewater biochemical system for treatment. The invention uses the water pipe as the mixing-reacting device, has little investment, high detoxification efficiency and good economic and social benefits.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a pretreatment method for a coal gas water seal pipeline.
Background
Because the water seal water is in direct contact with the coal gas, the soluble harmful substances in the coal gas are continuously dissolved into the water. Therefore, the gas water seal water is wastewater with complex components and serious pollution, and mainly contains pollutants such as sulfide, cyanide, phenol, ammonia nitrogen and the like. The pollutants in the gas water seal water, such as sulfide, cyanide, phenol, tar and the like are mostly cancerogenic substances, the degradation speed is slower in a natural state, and the biological hazard is great.
The water seal water of the gas of the steel and iron combined enterprises is produced in coke ovens, blast furnaces, converters and other operation units using gas, and the concentration of organic matters, ammonia nitrogen, total nitrogen, phenol, cyanide and sulfide in the wastewater is high, and the BOD/COD ratio is low. For example, in the gas seal water of a certain steel mill, COD is 4850mg/L, NH 4 + -N580 mg/L, TN 2000mg/L, phenol 400mg/L, cyanide 60mg/L, sulfide 60mg/L; while BOD/COD is only 0.05.
The gas water seal water is intermittently discharged and needs to be conveyed to a coking wastewater treatment station for centralized treatment by a pipeline. The distance from the production place of large-scale steel-iron combined enterprise gas water seal water to the coking wastewater treatment station is between 1 and 5 km. The waste water has great biotoxicity and directly enters a biochemical system for treatment, and serious impact is generated on the biochemical treatment system. Coking wastewater treatment is one of the key links of water pollution control in the steel industry, and the discharge of water seal water has serious influence on the stable operation of a coking wastewater biochemical treatment system. Therefore, the coal gas water seal pretreatment detoxification is very important.
In the paper EO+A2O2+BZ process for treating phenol-cyanogen wastewater (fuel and chemical industry, 2021, 52 (1)), gas water seal water is pretreated by electrochemistry, and then is treated by a biochemical system. The electrochemical pretreatment has higher efficiency, but the concentration of corrosive ions in the gas seal water is higher, and the service life of the anode material is greatly and negatively influenced. In addition, the electrochemical pretreatment facilities occupy large area and have large investment, and the factors also influence the popularization and application of the technology.
In the paper, "coke-blast furnace slag adsorption method for treating gas water seal water" (Shandong metallurgy, 1998,20 (2)), the gas water seal water is treated by utilizing the adsorption of coke and blast furnace slag, but the pollutants such as sulfide, cyanide, phenol, ammonia nitrogen and the like in the wastewater can be removed, the coke and the blast furnace slag need to be replaced and regenerated periodically.
In the paper 'chemical oxidation method is applied to treat wet gas tank water seal water' (metallurgical power, 2001, (3)), clO is utilized 2 ClO produced by a regenerator 2 The pollution degree of the gas water seal water is lower, and the significance of treating the heavy polluted gas water seal water is low; in addition, this technique requires the investment in ClO 2 The cost of the regenerator is high.
Therefore, the pretreatment detoxification technology with simple process, small occupied area and small investment is important for the treatment of the gas water seal water. The presently disclosed technology does not achieve these objectives well.
Disclosure of Invention
The embodiment of the invention provides a pretreatment method for a coal gas water seal pipeline, which realizes detoxification of the coal gas water seal pipeline by utilizing a catalytic composite oxidation technology in the pipeline conveying process of wastewater and improves the biodegradability of the wastewater.
The embodiment of the invention adopts the following technical scheme:
a pretreatment method of a coal gas water seal pipeline comprises the following steps:
s1: preparing a catalyst;
s2: the wastewater and ozone are sent into a micro-nano bubble generator for mixing, so that the ozone exists in the wastewater in a micro-nano bubble form, and the wastewater is output from a water outlet after the mixing is finished;
s3: adding a catalyst and a persulfate oxidizer into the wastewater;
s4: delivering the wastewater to a pipeline static mixer, and oxidizing the wastewater in the pipeline for 15-40 min;
s5: the catalyst is recycled, and the catalyst in the wastewater is recycled, so that the catalyst can be reused later, and the use cost is reduced;
s6: delivering the pretreated wastewater to a coking wastewater biochemical treatment system for subsequent treatment, wherein the coking wastewater/coal gas water seal water is output in a mode of more than or equal to 2/1;
further, the preparation steps of the catalyst are as follows:
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 ·6H 2 O and 10mmol Fe (NO) 3 ) 3 ·9H 2 O is dissolved in 100mL distilled water, and 100-mesh powdered activated carbon is added into the solution according to the molar ratio of AC to Mn to Fe of 200:1:2; stirring for 2-4 h at 500-800 ppm; slowly dripping NaOH solution with the concentration of 2mol/L until the pH value reaches 12;
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 8-12 h at 160-200 ℃;
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; and then drying the solid at the temperature of 100 ℃ to prepare the magnetic active carbon catalyst loaded with nano manganese ferrite.
Further, the persulfate oxidizer is potassium persulfate or sodium persulfate.
Further, ozone and gas water seal water are connected into a micro-nano bubble generator, and the average diameter of the generated micro-nano bubble ozone is less than or equal to 80 mu m.
Further, in the catalyst recovery and regeneration process, the catalyst in the wastewater is recovered through a magnetic device, then the residual magnetism in the catalyst is eliminated through a demagnetizer, and after washing for 5-8 times through deionized water and absolute ethyl alcohol, the catalyst is regenerated, and the regenerated catalyst can be highly dispersed in water and can keep the catalytic activity.
Further, the catalyst and the oxidant are used in the following amounts: catalyst 0.4-1.5 kg/m3; persulfate oxidizer 2.0-10.0 mM; ozone 0.3-1.0 kg/m3.
The above at least one technical scheme adopted by the embodiment of the invention can achieve the following beneficial effects:
firstly, the active carbon catalyst loaded with nano manganese ferrite, persulfate oxidant and micro-nano bubble ozone are added into water, and after being mixed by a pipeline static mixer, the active carbon catalyst reacts for 15-40 min, so that the molecular structure of toxic substances in the wastewater is destroyed, the biotoxicity of the toxic substances is reduced, the BOD/COD of the wastewater is raised to more than 0.25 after pretreatment, and the wastewater can directly enter a coking wastewater biochemical system for treatment.
Secondly, the invention uses the water pipe as a mixing-reacting device, thus the investment is small and the occupied area is small; because the active carbon in the catalyst has double functions of adsorption and catalysis, fe in the nano manganese ferrite 2+ /Fe 3+ And Mn of 2+ /Mn 3+ The cyclic activation catalysis is performed, the synergistic effect between the activated carbon and the nano manganese ferrite and the synergistic effect between the persulfate and the micro-nano bubble ozone are performed, and the detoxification efficiency of the wastewater is high under the action of various factors; the catalyst can be regenerated and reused. The popularization and application have good economic and social benefits.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a limitation on the invention. In the drawings:
FIG. 1 is an overall process flow diagram of the present invention;
FIG. 2 is a flow chart of a catalyst preparation process.
Description of the embodiments
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention and corresponding drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following describes in detail the technical solutions provided by the embodiments of the present invention with reference to the accompanying drawings.
The embodiment of the invention provides a pretreatment method of a coal gas water seal pipeline, which comprises the following steps:
s1: preparing a catalyst;
s2: the wastewater and ozone are sent into a micro-nano bubble generator for processing, and the wastewater and the ozone are output from a water outlet after the processing is completed;
s3: adding a catalyst and sodium persulfate into the wastewater and ozone;
s4: delivering the wastewater into a pipeline static mixer, oxidizing the wastewater in the pipeline for 15-40 min, and increasing BOD/COD of the outlet wastewater from 0.05 to above 0.25;
s5: the catalyst is recycled, and the catalyst in the wastewater is recycled, so that the catalyst can be reused later, and the use cost is reduced;
s6: and conveying the pretreated wastewater to a coking wastewater biochemical treatment system for subsequent treatment, wherein the coking wastewater/coal gas water seal water is output in a mode of more than or equal to 2/1.
The preparation steps of the catalyst are as follows:
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 ·6H 2 O and 10mmol Fe (NO) 3 ) 3 ·9H 2 O is dissolved in 100mL of distilled water, and the molar ratio of AC to Mn to Fe is 200:1:2,adding 100 mesh powdered activated carbon into the solution; stirring for 2-4 h at 500-800 ppm; then, slowly dripping NaOH solution (the concentration is 2 mol/L) until the pH value reaches 12;
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 8-12 h at 160-200 ℃;
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; drying the solid at 100 ℃ to prepare a magnetic active carbon catalyst loaded with nano manganese ferrite;
examples
1. Catalyst preparation step
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 •6H 2 O and 10mmol Fe (NO) 3 ) 3 •9H 2 O is dissolved in 100mL of distilled water, and 100-mesh powdered activated carbon is added into the solution according to the molar ratio of AC to Mn to Fe of 200:2:1; stirring for 4h at 500 rpm; then, naOH solution was slowly added dropwise to a pH of 12 at a concentration of 2 mol/L.
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 12 hours at 160 ℃.
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; and then drying the solid at the temperature of 100 ℃ to prepare the magnetic active carbon catalyst loaded with nano manganese ferrite.
2. Catalyst and oxidant addition
The gas water seal water and ozone enter a micro-nano bubble generator, the effluent enters a pipeline static mixer, and simultaneously the catalyst and sodium persulfate are added, so that the concentration of the catalyst, the sodium persulfate and the ozone in the water are respectively 0.5kg/m 3 、3.0mM、0.5kg/m 3 The pH value of the wastewater is 8; after the wastewater was oxidized in the pipeline for 20min, the COD of the outlet wastewater was reduced from 2174mg/L to 1513mg/L and the BOD/COD was increased from 0.05 to 0.26.
3. Catalyst recovery and regeneration
After the wastewater flows out of the pipeline, a magnetic device is used for recycling the catalyst in the water, and a demagnetizer is used for eliminating residual magnetism in the catalyst; and washing with deionized water and absolute ethyl alcohol for 5-8 times to realize catalyst regeneration. The regenerated catalyst can be highly dispersed in water and maintain catalytic activity.
4. Waste water treatment
The gas sealing water pretreated by the pipeline enters a coking wastewater biochemical treatment system according to the mode that the coking wastewater/gas sealing water is more than or equal to 2/1.
Examples
The preparation method of the catalyst and the pretreatment method of the water-sealed water pipeline of the coal gas comprise the following steps:
1. catalyst preparation step
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 6H2O and 10mmol Fe (NO) 3 ) 3 ·9H 2 O is dissolved in 100mL of distilled water, and 100-mesh powdered activated carbon is added into the solution according to the molar ratio of AC to Mn to Fe of 200:2:1; stirring for 4h at 500 rpm; thereafter, naOH solution (concentration: 2 mol/L) was slowly added dropwise thereto to a pH value of 12.
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 12 hours at 160 ℃.
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; and then drying the solid at the temperature of 100 ℃ to prepare the magnetic active carbon catalyst loaded with nano manganese ferrite.
2. Catalyst and oxidant addition
The water seal water and ozone of the coal gas enter a micro-nano bubble generator, the effluent enters a pipeline static mixer, and simultaneously, a catalyst and sodium persulfate are added, so that the concentrations of the catalyst, the sodium persulfate and the ozone in the water are respectively 1.5kg/m < 3 >, 6.0mM, 0.7kg/m < 3 >, and the pH value of the wastewater is 8; after the wastewater is oxidized in the pipeline for 30min, the COD of the outlet wastewater is reduced from 4956mg/L to 3765mg/L, and the BOD/COD is increased from 0.05 to 0.30.
3. Catalyst recovery and regeneration
After the wastewater flows out of the pipeline, a magnetic device is used for recycling the catalyst in the water, and a demagnetizer is used for eliminating residual magnetism in the catalyst; and washing with deionized water and absolute ethyl alcohol for 5-8 times respectively to realize catalyst regeneration. The regenerated catalyst can be highly dispersed in water and maintain catalytic activity.
4. Waste water treatment
The gas sealing water pretreated by the pipeline enters a coking wastewater biochemical treatment system according to the mode that the coking wastewater/gas sealing water is more than or equal to 2/1.
Examples
The preparation method of the catalyst and the pretreatment method of the water-sealed water pipeline of the coal gas comprise the following steps:
1. catalyst preparation step
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 6H2O and 10mmol Fe (NO) 3 ) 3 ·9H 2 O is dissolved in 100mL of distilled water, and 100-mesh powdered activated carbon is added into the solution according to the molar ratio of AC to Mn to Fe of 200:2:1; stirring for 4h at 500 rpm; thereafter, naOH solution (concentration: 2 mol/L) was slowly added dropwise thereto to a pH value of 12.
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 8 hours at 180 ℃.
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; and then drying the solid at the temperature of 100 ℃ to prepare the magnetic active carbon catalyst loaded with nano manganese ferrite.
2. Catalyst and oxidant addition
The water seal water and ozone of the coal gas enter a micro-nano bubble generator, the effluent enters a pipeline static mixer, and simultaneously, a catalyst and sodium persulfate are added, so that the concentrations of the catalyst, the sodium persulfate and the ozone in the water are respectively 1.0kg/m3, 5.0mM and 1.0kg/m3, and the pH value of the wastewater is 8; after the wastewater is oxidized in the pipeline for 40min, the COD of the outlet wastewater is reduced from 4954mg/L to 3652mg/L, and the BOD/COD is increased from 0.05 to 0.32.
3. Catalyst recovery and regeneration
After the wastewater flows out of the pipeline, a magnetic device is used for recycling the catalyst in the water, and a demagnetizer is used for eliminating residual magnetism in the catalyst; and washing with deionized water and absolute ethyl alcohol for 5-8 times respectively to realize catalyst regeneration. The regenerated catalyst can be highly dispersed in water and maintain catalytic activity.
4. Waste water treatment
The gas sealing water pretreated by the pipeline enters a coking wastewater biochemical treatment system according to the mode that the coking wastewater/gas sealing water is more than or equal to 2/1.
The foregoing is merely exemplary of the present invention and is not intended to limit the present invention. Various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are to be included in the scope of the claims of the present invention.
Claims (5)
1. The pretreatment method of the gas water seal pipeline is characterized by comprising the following steps of:
s1: preparing a catalyst;
s2: feeding the gas water seal water and ozone into a micro-nano bubble generator for mixing, so that the ozone exists in the gas water seal water in a micro-nano bubble mode, and outputting the mixed gas water seal water from a water outlet;
s3: adding a catalyst and a persulfate oxidizer into the water discharged in the step S2;
s4: delivering the S3 effluent to a pipeline static mixer, and oxidizing for 15-40 min in a pipeline;
s5: the catalyst is recycled, and the catalyst in the S4 effluent is recycled, so that the catalyst can be reused later, and the use cost is reduced;
s6: the pretreated coal gas water seal water is conveyed to a coking wastewater biochemical treatment system for subsequent treatment, wherein the coking wastewater/coal gas water seal water is output in a mode of more than or equal to 2/1;
the preparation steps of the catalyst are as follows:
(1) Mixing and stirring: 5mmol Mn (NO) 3 ) 2 ·6H 2 O and 10mmol Fe (NO) 3 ) 3 ·9H 2 O is dissolved in 100mL of distilled water, and 100-mesh powdered activated carbon is added into the solution according to the molar ratio of AC to Mn to Fe of 200:1:2; stirring for 2-4 h at 500-800 ppm; slowly dripping NaOH solution with the concentration of 2mol/L until the pH value reaches 12;
(2) Hydrothermal reaction: adding the mixed solution obtained in the step (1) into an autoclaved reaction kettle, and reacting for 8-12 h at 160-200 ℃;
(3) Washing and drying: separating solid from the hydrothermal reaction solution, and repeatedly washing with distilled water until the pH value of the washing solution is reduced to 7; and then drying the solid at the temperature of 100 ℃ to prepare the magnetic active carbon catalyst loaded with nano manganese ferrite.
2. The pretreatment method of a gas water sealed pipeline according to claim 1, wherein the persulfate oxidizer is potassium persulfate or sodium persulfate.
3. The pretreatment method of a gas water seal pipeline according to claim 1, wherein ozone and gas water seal water are connected into a micro-nano bubble generator for mixing, and the average diameter of the generated micro-nano bubble ozone is less than or equal to 80 μm.
4. The pretreatment method of the gas water-sealed water pipeline according to claim 1, wherein in the catalyst recovery and regeneration process, the catalyst in the effluent is recovered through a magnetic device, then the residual magnetism in the catalyst is eliminated through a demagnetizer, and after washing for 5-8 times through deionized water and absolute ethyl alcohol, the catalyst is regenerated, and the regenerated catalyst can be highly dispersed in water and can keep the catalytic activity.
5. The pretreatment method of the gas water-sealed water pipeline according to claim 1, wherein the dosage of the catalyst and the oxidant is as follows: catalyst 0.4-1.5 kg/m 3 The method comprises the steps of carrying out a first treatment on the surface of the Persulfate oxidizer 2.0-10.0 mM; ozone 0.3-1.0 kg/m 3 。
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