CN110606539B - Method for treating organic wastewater by utilizing sludge resource - Google Patents

Method for treating organic wastewater by utilizing sludge resource Download PDF

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CN110606539B
CN110606539B CN201910983174.7A CN201910983174A CN110606539B CN 110606539 B CN110606539 B CN 110606539B CN 201910983174 A CN201910983174 A CN 201910983174A CN 110606539 B CN110606539 B CN 110606539B
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sludge
catalyst
wastewater
organic wastewater
sewage treatment
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CN110606539A (en
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寇丽栋
王静
赵亮
田振邦
王俊
段文杰
曹继红
黄做华
黄伟庆
李宾宾
李箐湲
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Institute of Chemistry Henan Academy of Sciences Co Ltd
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • 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
    • 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
    • C02F2101/30—Organic compounds
    • 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
    • C02F2209/20—Total organic carbon [TOC]

Abstract

The invention discloses a method for treating organic wastewater by sludge resource utilization, belonging to the field of sludge resource utilization and the technical field of water treatment. The invention utilizes concentrated pond sludge (containing Fenton advanced treatment sludge) generated by a papermaking sewage treatment plant and an industrial park sewage treatment plant as a raw material, and KMnO is added4And (3) carrying out conditioning reaction, and then carrying out dehydration, cleaning, drying, crushing and high-temperature roasting to prepare the sludge carbon-based Fe-Mn catalyst. The prepared catalyst is used for treating the refractory organic wastewater in the presence of Peroxymonosulfate (PMS), thereby realizing the win-win of sludge resource utilization and high-efficiency removal of the refractory wastewater. The preparation method of the catalyst has the advantages of low-cost and easily-obtained raw materials, simple preparation process, waste utilization, sludge dehydration performance improvement and TOC removal of wastewater generated by sludge dehydration.

Description

Method for treating organic wastewater by utilizing sludge resource
Technical Field
The invention relates to a method for treating organic wastewater by sludge resource utilization, belonging to the field of sludge resource utilization and the technical field of water treatment.
Background
Sludge is an unavoidable byproduct in the sewage treatment process, usually contains pathogenic microorganisms, parasitic ova and a large amount of refractory substances, and causes environmental pollution if the treatment is not thorough. At present, the treatment and disposal of a large amount of sludge generated by water treatment are problems which are difficult to solve at home. The COD transferred from the sewage to the sludge accounts for about 30-50%, the nitrogen transferred to the sludge accounts for about 20-30%, and the phosphorus accounts for about 90%. If the sludge is not reasonably treated, the aims of energy conservation and emission reduction are greatly discounted, so that the sewage treatment and the sludge are repeated. How to properly treat the sludge to stabilize, make the sludge harmless, reduce and recycle the sludge becomes an important problem in environmental management. At present, the main methods for treating sludge in China comprise landfill, composting, natural drying and incineration, and the sanitary landfill needs to occupy a large amount of land resources and is very easy to pollute the ecological environment; the compost can realize the resource utilization of the sludge, but the heavy metal in the sludge becomes a bottleneck; the paying incineration and drying technology consumes more energy, and the incineration easily causes air pollution. Therefore, the resource utilization of the sludge is great and imperative.
However, the existing biological treatment method is difficult to treat substances with poor biodegradability and relative molecular mass from thousands to tens of thousands, and the Advanced Oxidation Process (AOPs) can directly mineralize or oxidize the high-concentration organic wastewater based on the generation of high-activity oxygen species such as hydroxyl radicals, superoxide anion radicals, sulfate radicals and singlet oxygen, can completely mineralize or decompose most organic substances, improves the biodegradability of pollutants, has great advantages in the treatment of trace harmful chemical substances such as environmental hormones and the like, and has good application prospects. Hydrogen peroxide and persulfates are common oxidants in AOPs that generate active oxygen. Persulfates, e.g. peroxomonosulfate (PMS, HSO)5 -) And peroxodisulfate (PDS, S)2O8 2-) Due to the specific ratio of hydrogen peroxide (H)2O2) More stable, persulfate activation processSulfate radical (E) produced in (1)0= 2.5-3.1V) is more selective than hydroxyl (E0 = 1.8-2.7V), and compounds having a carbon-carbon double bond and a benzene ring can be oxidized, attracting increasing attention of researchers. While the persulfate can be activated by heat radiation, ultraviolet, transition metals, cations and zero-valent metals, but high-temperature and ultraviolet radiation have higher requirements on energy, and the toxicity and secondary pollution risks of some metals restrict the further application of the activation methods in industry, so that the development of the catalyst activated persulfate with low cost, high efficiency and strong stability has important significance for degrading organic pollutants.
The sludge has high organic matter content and contains various metal elements, the peat can be prepared by physical and chemical methods, and the like, and the Mn metal with high activity and difficult loss is loaded on the peat to prepare the catalyst for treating the organic wastewater difficult to degrade, so that the purpose of treating wastes with processes of wastes against one another is achieved, the sludge resource utilization is realized, and the environmental protection is facilitated. At present, no relevant report is found.
Disclosure of Invention
The invention aims to provide a method for treating organic wastewater by recycling sludge, which is used for preparing a sludge-based metal catalyst by using the sludge, degrading pollutants in the organic wastewater, realizing the treatment of waste by waste and realizing industrial popularization and application.
In order to achieve the aim, the invention takes the sludge of the concentration tank and active components as carriers and KMnO4Is a conditioner, and a manganese-containing substance generated after the oxidation degradation of the conditioner is used as an active component to prepare the sludge carbon-based Fe-Mn catalyst which is used for treating organic wastewater.
The specific method comprises the following steps: (1) and (3) adding potassium permanganate into the sludge in the concentration tank, and stirring and mixing uniformly. (2) And (2) filtering the mud completely reacted in the step (1), washing the mud with deionized water, and drying and grinding a filter cake. (3) Placing the precursor obtained in step (2) in a crucible at 600oC-900 oAnd C, roasting at high temperature, and cooling to room temperature after the roasting is finished to obtain the sludge carbon-based Fe-Mn catalyst. (4) Adding the obtained sludge carbon-based Fe-Mn catalyst into the organic wastewater difficult to degrade,then adding a peroxymonosulfate oxidant to degrade and mineralize organic matters in the wastewater. The treatment condition is that the reaction temperature is 10-45 DEG CoC, pH: 2 to 12, 1 to 5mmol/L of Peroxymonosulfate (PMS), 0.1 to 1.0g/L of sludge carbon-based Fe-Mn catalyst and 0.01 to 0.5mmol/L of hardly degradable organic matter.
The adopted sludge of the concentration tank is mainly from a papermaking sewage treatment plant or an industrial park sewage treatment plant, the content of organic matters of absolute dry sludge is 50-60%, the water content of the sludge is 90-99%, and the ash contains elements such as calcium, iron, silicon, aluminum and the like, wherein the mass percentage of the iron element is 8-10%. The KMnO4The optimal adding amount is 7 to 20 percent of the weight of the absolutely dry sludge.
The peroxymonosulfate oxidizing agent is preferably oxone or sodium persulfate.
The invention has the innovation points that: uses the sewage peat as a framework, utilizes iron element in the sludge, and adds KMnO4And preparing the sludge carbon-based catalyst containing iron and manganese for catalyzing and degrading organic wastewater.
The invention has the following advantages:
Figure 441178DEST_PATH_IMAGE001
the iron-containing sludge is fully utilized and is taken as a main raw material, and KMnO is added4The novel sludge carbon-based catalyst is obtained after pretreatment and firing, is used for treating organic wastewater difficult to degrade, can efficiently and quickly remove organic pollutants in a water body, provides a way for sludge treatment, and accords with the concept of sustainable development and the national energy-saving and emission-reducing policy.
Figure 521129DEST_PATH_IMAGE002
The invention simultaneously improves the sludge dewatering performance and efficiently removes TOC in the wastewater generated by sludge dewatering.
Figure 937067DEST_PATH_IMAGE003
The iron-containing sludge and Mn in the potassium permanganate added in the pretreatment have synergistic effect, can efficiently degrade and even mineralize organic matters which are difficult to degrade in the wastewater, has good effect in a strong acid and strong alkali reaction system, and can be circularly usedThe catalyst has the same catalytic efficiency after calcination after 5 times of use and 5 times of recycling. The problems of poor stability, insufficient catalytic performance, high cost and the like of the traditional catalyst are solved, and the catalyst is high in efficiency and strong in activity and is excellent in performance. Is beneficial to the popularization and the application in the wastewater treatment, and has good environmental benefit and economic benefit.
Drawings
FIG. 1 shows the shape and microstructure of the catalyst prepared in the examples of the present invention, a is untreated direct firing and b is treated post firing.
FIG. 2 is a schematic diagram of the analysis of the binding energy of C, O, N, Fe and Mn in the catalyst of the present invention by X-ray photoelectron spectroscopy.
FIG. 3 shows the removal and mineralization rates of phenol for catalysts fired at different conditioner additions.
Detailed Description
The sludge carbon-based Fe-Mn catalyst provided by the invention can be used for treating organic wastewater difficult to degrade, can improve the removal rate of organic matters and promotes the wide application of catalytic oxidation technology. The present invention is described in detail below with reference to examples and the accompanying drawings.
Comparative example 1:
Figure 735259DEST_PATH_IMAGE001
taking sludge in a concentration tank after Fenton advanced treatment in a certain paper mill, wherein the mass percentage of iron element is 8-10%, and adding KMnO according to 0% of the weight of absolute dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 30min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 465317DEST_PATH_IMAGE002
The composite catalyst precursor was placed under vacuum at 600 deg.CoC (rate of temperature rise 10)oC/min) roasting for 2h, and then naturally cooling to room temperature under a vacuum state to obtain the black peat-based catalyst.
Figure 134196DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the black peat-based catalyst is 0.5g/L, the concentration of phenol is 30mg/L, the addition amount of oxone is 3mmol/L, and the reaction temperature is 25oC, pH =4, the rotation speed of a shaker is 150r/min, the reaction time is 90min, the conversion rate of phenol is 72.3%, and the removal rate of TOC is 39.6%.
Example 1:
Figure 924297DEST_PATH_IMAGE001
taking sludge in a concentration tank after Fenton advanced treatment in a certain paper mill, wherein the mass percentage of iron element is 8-10%, and adding KMnO according to 4% of the weight of the absolutely dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 40min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 209785DEST_PATH_IMAGE002
The composite catalyst precursor was placed under vacuum at 700 deg.CoC (rate of temperature rise 5)oC/min) roasting for 3 h, and then naturally cooling to room temperature in a vacuum state to obtain the black peat based Fe-Mn catalyst.
Figure 274693DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =4, the rotation speed of a shaker is 150r/min, the reaction time is 90min, the phenol conversion rate is 86.5%, and the TOC removal rate is 63.9%.
Example 2:
Figure 329237DEST_PATH_IMAGE001
after a certain paper mill Fenton is taken for deep treatmentThe concentrated pond sludge of (1), wherein the iron element accounts for 8-10% by mass, and KMnO is added according to 7% of the weight of the absolutely dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 50min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 290240DEST_PATH_IMAGE002
The composite catalyst precursor is placed under vacuum at 800 deg.CoC (rate of temperature rise 10)oC/min) roasting for 4 h, and then naturally cooling to room temperature in a vacuum state to obtain the black peat based Fe-Mn catalyst.
Figure 531865DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =4, the rotation speed of a shaker is 150r/min, the reaction time is 90min, the phenol conversion rate is 96.2%, and the TOC removal rate is 71.9%.
Example 3:
Figure 603726DEST_PATH_IMAGE001
taking sludge in a concentration tank after Fenton advanced treatment in a certain paper mill, wherein the mass percentage of iron element is 8-10%, and adding KMnO according to 10% of the weight of the absolutely dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 60 min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 778356DEST_PATH_IMAGE002
The composite catalyst precursor is placed under vacuum at 900 deg.CoC (rate of temperature rise 10)oC/min) roasting for 2h, and then naturally cooling to room temperature in a vacuum state to obtain black mudCarbon-based Fe-Mn catalyst.
Figure 647610DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =10, the rotation speed of a shaker is 150r/min, the reaction time is 90min, the conversion rate of phenol is 97.5%, and the removal rate of TOC is 71.9%.
Example 4:
Figure 704428DEST_PATH_IMAGE001
taking sludge in a concentration tank after Fenton advanced treatment in a certain paper mill, wherein the mass percentage of iron element is 8% -10%, adding KMnO4 according to 13% of the weight of the absolutely dry sludge, stirring and mixing uniformly by magnetic force, reacting for about 30min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oDrying in a forced air drying oven of CoC, and grinding to obtain the composite catalyst precursor.
Figure 314401DEST_PATH_IMAGE002
The composite catalyst precursor was placed under vacuum at 600 deg.CoC (rate of temperature rise 10)oC/min) roasting for 2h, and then naturally cooling to room temperature in a vacuum state to obtain the black peat based Fe-Mn catalyst.
Figure 343537DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =10, the rotation speed of a shaker is 150r/min, the reaction time is 90min, the conversion rate of phenol is 95.1%, and the removal rate of TOC is 66.8%.
Example 5:
Figure 115184DEST_PATH_IMAGE001
taking sludge in a concentration tank after Fenton advanced treatment in a certain paper mill, wherein the mass percentage of iron element is 8-10%, and adding KMnO according to 16% of the weight of the absolutely dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 30min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 862560DEST_PATH_IMAGE002
The composite catalyst precursor was placed under vacuum at 600 deg.CoC (rate of temperature rise 10)oC/min) roasting for 2h, and then naturally cooling to room temperature in a vacuum state to obtain the black peat based Fe-Mn catalyst.
Figure 276224DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =12, the rotating speed of a shaker is 150r/min, the reaction time is 90min, the phenol conversion rate is 96.3%, and the TOC removal rate is 72.1%.
Example 6:
Figure 159866DEST_PATH_IMAGE001
taking sludge in a concentration tank treated by a sewage treatment plant in an industrial park, wherein the mass percentage of iron element is 8-10%, and adding KMnO according to 20% of absolute dry sludge4And (3) uniformly mixing by magnetic stirring, reacting for about 30min completely, and performing suction filtration and water washing to obtain a filter cake. Placing the filter cake in 105oAnd C, drying in a blast drying oven, and grinding to obtain the composite catalyst precursor.
Figure 633573DEST_PATH_IMAGE002
The composite catalyst precursor was placed under vacuum at 600 deg.CoC (rate of temperature rise 10)oC/min) Roasting for 2h, and naturally cooling to room temperature in a vacuum state to obtain the black peat based Fe-Mn catalyst.
Figure 602666DEST_PATH_IMAGE003
Advanced catalytic oxidation experimental conditions: the addition amount of the Fe-Mn sludge activated carbon catalyst is 0.5g/L, the phenol concentration is 30mg/L, the addition amount of the potassium hydrogen persulfate is 3mmol/L, and the reaction temperature is 25oC, pH =7, the rotating speed of a shaker is 150r/min, the reaction time is 90min, the phenol conversion rate is 100%, and the TOC removal rate is 80.2%.

Claims (1)

1. A method for treating organic wastewater by utilizing sludge resources is characterized by comprising the following steps: (1) taking sludge in a concentration tank, adding potassium permanganate, and stirring and mixing uniformly; (2) filtering the mud completely reacted in the step (1), washing the mud with deionized water, and drying and grinding a filter cake; (3) placing the precursor obtained in step (2) in a crucible at 600oC-900 oC, roasting at high temperature, and cooling to room temperature after the roasting is finished to obtain the sludge carbon-based Fe-Mn catalyst; (4) adding the obtained sludge carbon-based Fe-Mn catalyst into refractory organic wastewater, and then adding a peroxymonosulfate oxidant to degrade and mineralize organic matters in the wastewater;
the adopted sludge of the concentration tank comes from a paper-making sewage treatment plant or an industrial park sewage treatment plant, wherein the mass percentage of the iron element is 8-10 percent; the KMnO4The adding amount is 7 to 20 percent of the weight of the absolutely dry sludge;
the treatment condition of the step (4) is that the reaction temperature is 10-45 DEG CoC, pH: 2 to 12, the addition amount of the peroxymonosulfate is 1 to 5mmol/L, the addition amount of the sludge carbon-based Fe-Mn catalyst is 0.1 to 1.0g/L, and the concentration of the refractory organic matter is 0.01 to 0.5 mmol/L.
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CN111437825B (en) * 2020-05-28 2023-06-20 广东工业大学 Iron-manganese biochar catalyst and application thereof in conditioning sludge dewatering
CN114308039A (en) * 2022-01-06 2022-04-12 昆明华信金属材料制造有限公司 Rolling mill sludge recycling method
CN114534772B (en) * 2022-01-17 2023-07-25 西华大学 Catalyst for antibiotic wastewater treatment and application thereof

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CN106540672A (en) * 2016-12-07 2017-03-29 合肥学院 A kind of magnetic porous sludge carbon carries metal oxide catalyst and its reacts the application in degraded azo dye in persulfate oxidation
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