CN108002547B - Coal chemical industry wastewater advanced treatment method based on living cell immobilization technology - Google Patents
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Abstract
The invention discloses a coal chemical industry wastewater advanced treatment method based on living cell immobilization technology, which comprises the following steps: (1) the wastewater is derived from coal chemical wastewater after pretreatment such as oil removal, dephenolization, ammonia blowing and the like, anaerobic digestion and aerobic biochemical treatment, the water quality of the wastewater does not reach the standard, and refractory substances such as polycyclic aromatic hydrocarbon, nitrogen-containing heterocycle and the like still exist. (2) Aiming at refractory organic matters, a polyvinyl alcohol (PVA) water-absorbing sponge material modified by nano copper oxide is used as a carrier, the refractory organic matters are used for domesticating and screening dominant flora, advanced treatment is carried out on coal chemical industry wastewater by a biochemical method based on a living cell immobilization technology, the immobilized flora is found to have stable and efficient degradation performance on the organic matters which are difficult to remove by a common biochemical treatment method, finally, the harmless treatment of the coal chemical industry wastewater is realized, and a beneficial reference is provided for actual wastewater treatment.
Description
Technical Field
The invention belongs to the technical field of sewage and wastewater treatment, and particularly relates to a coal chemical industry wastewater advanced treatment method based on a living cell immobilization technology.
Background
The coal chemical industry has brought about great environmental problems while developing rapidly. The coal chemical engineering project has huge water demand, and no matter the traditional coal chemical engineering or the novel coal chemical engineering, a large amount of industrial wastewater can be generated in the production process of the coal chemical engineering project, wherein the industrial wastewater comprises coking wastewater, semi-coke wastewater, coal gasification and coal liquefaction production wastewater and the like, the wastewater contains various toxic and harmful pollutants such as phenol, ammonia nitrogen, petroleum hydrocarbon, polycyclic aromatic hydrocarbon, nitrogen-containing heterocyclic rings, cyanides and the like, the components are complex, the concentration is high, the toxicity is high, the property is stable, the coal chemical engineering project belongs to high-concentration organic industrial wastewater which is difficult to be biochemically degraded, and the pollution control of the coal chemical engineering project is always a. The treatment and recycling technology of the coal chemical industry wastewater gradually becomes a bottleneck restricting the rapid development of the coal chemical industry, and the finding of an economic and effective wastewater treatment method has great significance.
The existing coal chemical wastewater treatment is generally that targeted physicochemical pretreatment is firstly carried out, then biological treatment is carried out, and finally advanced treatment is carried out. The pretreatment of waste water mainly comprises oil removal, dephenolization, ammonia distillation, suspended solid removal and the like, and the common biological treatment process comprises A2O, A/O, SBR, UASB, etc. The coal chemical industry waste water COD, ammonia nitrogen and phenol concentration are high, contain difficult degradation organic matter, in order to better handle this kind of waste water, general biochemical treatment process is difficult to reach ideal effect, goes out water COD because contain difficult degradation organic matter or other materials exist and can not reach discharge standard, consequently need carry out advanced treatment. The conventional advanced treatment methods comprise chemical coagulation, adsorption, advanced oxidation technology, membrane separation technology and the like, and the physical and chemical methods generally have the problems of high cost and maintenance cost, easy secondary pollution and the like, so that the search for more environment-friendly advanced treatment methods has great significance for treating wastewater in the coal chemical industry.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a coal chemical industry wastewater advanced treatment method based on a living cell immobilization technology, which is used for screening floras which efficiently utilize refractory organic matters, preparing immobilized cells by adopting the immobilization technology to carry out advanced treatment on wastewater, solving the problems of low degradation efficiency of a conventional biological treatment unit, poor effluent quality, high cost of a physical and chemical advanced treatment method, easy secondary pollution and the like in the coal chemical industry wastewater, and finally realizing the harmless treatment of the coal chemical industry wastewater.
In order to achieve the purpose, the invention adopts the technical scheme that:
a coal chemical industry wastewater advanced treatment method based on living cell immobilization technology comprises the following steps:
step 1, performing physicochemical pretreatment and conventional biochemical treatment on coal chemical wastewater; after the treatment of the step, refractory organic matters such as polycyclic aromatic hydrocarbon, volatile phenol and the like, such as quinoline, phenol, naphthalene and the like, still exist in the wastewater;
and 2, loading the domesticated dominant flora on a modified nano copper oxide (CuO NPs) -polyvinyl alcohol (PVA) based sponge carrier to prepare an immobilized flora, and further adsorbing and metabolizing the organic matters which are difficult to degrade in the step 1 by using the obtained immobilized flora to realize harmless discharge of wastewater.
The preparation method of the modified nano copper oxide (CuO NPs) -polyvinyl alcohol (PVA) -based sponge carrier comprises the following steps:
(1) pretreatment of PVA-based sponge: soaking and stirring the mixture for 20min to 30min by hydrochloric acid with the mass concentration of 5 percent to 8 percent, washing the mixture twice by pure water, soaking and stirring the mixture for 20min to 30min by sodium hydroxide with the mass concentration of 5 percent to 8 percent, washing the mixture by the pure water until the pH value is 6 to 8, soaking and ultrasonically treating the mixture for 1h to 2h by the pure water, and drying the mixture at the temperature of between 50 and 60 ℃;
(2) preparing a modified nano copper oxide (CuO NPs) -polyvinyl alcohol (PVA) based sponge carrier: adding 0.2g-0.3g of pretreated PVA-based sponge into 80mL-150mL of nano copper oxide solution with the concentration of 50mg/L-150mg/L, fully mixing in an ultrasonic reactor for 30min-40min, separating out the PVA-based sponge loaded with CuO NPs, and carrying out vacuum drying at 50-60 ℃ for 10-15 h to obtain the nano copper oxide-polyvinyl alcohol-based sponge material.
The domestication method of the dominant flora comprises the following steps:
taking activated sludge as a bacteria source, adding tap water for dilution, carrying out aerobic culture at room temperature, standing, taking supernatant, inoculating the supernatant into a culture medium for culture and enrichment, cleaning bacteria by using sterilized inorganic salt after enrichment, simultaneously adding the bacteria into an inorganic salt culture medium for acclimatization culture, taking the organic matters difficult to degrade as a carbon source, inoculating and repeatedly acclimatizing, monitoring the condition of degrading the organic matters by the bacteria by taking TOC of a system as an index, and finally separating and purifying by adopting a plate scribing method to obtain a flora with a degradation effect meeting the requirement.
The mass ratio of the tap water to the activated sludge is 1:1, the aerobic culture time is 24 hours, the DO concentration is 2.0-3.0mg/L, the culture medium is LB culture medium, the culture is 24 hours, the dosage of the supernatant is 15mL, and the supernatant is inoculated in 85mL of sterilized culture medium for culture and enrichment.
The inorganic salt culture medium comprises the following components: na (Na)2HPO4 4.26g/L，KH2PO4 2.65g/L，MgSO4·7H2O 0.20g/L，CaCl2 0.02g/L，MnSO4·7H2O 0.002g/L，(NH4)2SO40.4g/L and 1mL/L of trace elements, wherein the specific formula of the trace elements is as follows: FeCl2·4H2O 1.50g/L,CuCl2·2H2O0.002g/L,MnSO4·7H2O 0.10g/L,Na2MoO4·2H2O 0.024g/L,ZnCl2 0.006g/L,H3BO30.07g/L, adjusting pH of the culture medium to 7.0, sterilizing at 121 deg.C for 25min, and cooling.
The refractory organics are acclimatized repeatedly with 15% of inoculum size, and the initial concentration of each refractory organics is 20 mg.L-1At a concentration of 20 mg.L-1Gradually increased to a concentration of 200 mg/L.
The process for preparing the immobilized flora comprises the following steps:
enriching the separated dominant flora by using a culture medium, cleaning by using inorganic salt to prepare a bacterial suspension, weighing a certain amount of modified nano copper oxide (CuO NPs) -polyvinyl alcohol (PVA) -based sponge carrier, sterilizing at 121 ℃ for 25 minutes, cooling to room temperature after sterilization, adding the bacterial suspension into a reaction container, adding the organic matter which is difficult to degrade as a carbon source, carrying out aerobic culture, and monitoring the complete degradation of the organic matter by using TOC to finish the immobilization process of the flora.
And taking out the modified nano copper oxide (CuO NPs) -polyvinyl alcohol (PVA) -based sponge carrier with the immobilized flora, and slowly cleaning twice by using sterilized MSM to remove free bacteria on the surface for subsequent advanced treatment of the coal chemical industry wastewater.
The organic matter which is difficult to degrade is one or more of quinoline, phenol and naphthalene.
The culture medium is LB culture medium, the inorganic salt is MSM, OD600＝1.0±0.1, the solid-liquid ratio of the carrier to the bacterial suspension in the reaction vessel is 12-15g/L, the adding amount of single organic matter which is difficult to degrade is 100mg/L, wherein naphthalene is dissolved in acetone in advance.
Compared with the prior art, the method selects the novel PVA water-absorbing sponge material modified by nano copper oxide as the carrier to fix the dominant bacteria, utilizes the mixed organic matters to domesticate and screen the high-efficiency bacteria group for treating the organic matters difficult to degrade, the immobilized microorganisms have higher tolerance to the coal chemical industry wastewater, the better degradation effect can be achieved, the advanced treatment process of the microorganism method has no secondary pollution, and the final harmless treatment of the coal chemical industry wastewater is realized.
Detailed Description
The following examples are provided to explain embodiments of the present invention in detail.
Example 1
Wastewater generated by a certain semi-coke enterprise in northern Shaanxi is selected as a research object to carry out pretreatment resource recovery and biochemical treatment, and the water quality of raw water and the effluent quality of each stage of pretreatment and biochemical treatment are shown in the following table:
TABLE 1 blue waste water quality
| Treatment stage | COD(mg/L) | Ammonia nitrogen (mg/L) | Volatile phenol (mg/L) |
| Raw water | 31200 | 4250 | 3350 |
| Oil removal | 13450 | 4118 | 3314 |
| Dephenolation | 4170 | 4010 | 325 |
| Blowing ammonia | 3300 | 630 | 298 |
| Anaerobic digestion | 947 | 274 | 148 |
| Aerobic biochemical treatment | 174 | 38 | 53 |
After pretreatment and biochemical treatment, the final COD of the coal chemical wastewater is reduced to 174mg/L, the ammonia nitrogen is reduced to 38mg/L, the concentration of volatile phenol is 53mg/L and does not reach the standard, the main organic matter composition in the water is analyzed by using gas chromatography, and compared with standard substances, the detected substances are mainly shown in the following table:
TABLE 2 concentration of the main organics in the biochemical effluent
| Organic matter | Average concentration (mg/L) | Organic matter | Average concentration (mg/L) |
| Phenol and its preparation | 7.2 | Naphthalene | 46.5 |
| Ortho-cresol | 3.9 | Acenaphthylene | 4.3 |
| Meta, para-cresol | 12.7 | Fluorene compounds | 21.2 |
| 2, 4-dimethylphenol | 5.4 | Phenanthrene | 0.2 |
| 4-chloro-3-methylphenol | 2.1 | Quinolines | 3.3 |
| 2,4, 5-trichlorophenol | 10.9 | Isoquinoline derivatives | 1.1 |
| Pentachlorophenol | 0.8 | Indoles | 0.6 |
Under the condition of laboratory, the deep treatment is carried out by adopting the living cell activation technology.
Preparation of CuO NPs loaded PVA carrier
Soaking PVA-based sponge in 5% hydrochloric acid for 30min, washing with pure water twice, soaking in 5% sodium hydroxide for 30min, washing with pure water until pH is 7, soaking in pure water for ultrasonic treatment for 1 hr, and oven drying at 55 deg.C. Adding the pretreated PVA-based sponge into a solution containing nano copper oxide at a ratio of 2.5g/L, fully mixing the mixed solution in an ultrasonic reactor for 30min, separating out the PVA-based sponge loaded with CuO NPs, drying in vacuum at 60 ℃ for 12 h, and placing in a dry closed container for later use.
2. Screening and domestication of dominant flora of refractory organic matters
Taking activated sludge of a certain sewage treatment plant in Xian city as a bacteria source, adding tap water into a collected sample for dilution (the ratio is 1:1), and diluting at 30 ℃ for 180 r.min-1The shaking table incubator is used for constant-temperature culture for 24 hours, after standing, 15mL of supernatant is taken to be inoculated into 85mL of sterilized LB culture medium for culture for 24 hours for enrichment, after enrichment, bacteria are cleaned by using a sterilized inorganic salt culture medium, meanwhile, the bacteria are added into the inorganic salt culture medium for acclimatization culture, the mixture of quinoline, phenol and naphthalene is used as a carbon source, the acclimatization is carried out repeatedly according to 15 percent of inoculum concentration, and the initial concentrations of quinoline, phenol and naphthalene are respectively 20 mg.L-1At a concentration of 20 mg.L-1The gradient is gradually increased to the concentration of 200mg/L, the condition that bacteria degrade organic matters is monitored by taking the TOC of the system as an index, and finally, a flora with better degradation effect is obtained by separation and purification by a plate scribing method.
4. The inorganic salt culture medium in the step 3 comprises the following components: na (Na)2HPO4 4.26g/L，KH2PO4 2.65g/L，MgSO4·7H2O 0.20g/L，CaCl2 0.02g/L，MnSO4·7H2O 0.002g/L，(NH4)2SO40.4g/L and 1mL/L of trace elements, wherein the specific formula of the trace elements is as follows: FeCl2·4H2O 1.50g/L,CuCl2·2H2O 0.002g/L,MnSO4·7H2O 0.10g/L,Na2MoO4·2H2O 0.024g/L,ZnCl2 0.006g/L,H3BO30.07g/L, adjusting pH of the culture medium to 7.0, sterilizing at 121 deg.C for 25min, and cooling.
5. The immobilization process of the flora is as follows: selecting dominant organic matter degradation flora enriched and separated from LB culture medium, cleaning with inorganic salt, and preparing into OD600Bacterial suspension 1.0 ± 0.1. Weighing 3g of CuO NPs loaded PVA material, placing the material in a 500mL conical flask, sterilizing at 121 ℃ for 25 minutes, cooling to room temperature after sterilization, and adding 200mL of OD into the conical flask600Adding 100mg/L quinoline, 100mg/L phenol and 100mg/L naphthalene as carbon sources into the bacterial suspension of 1.0 +/-0.1, culturing at the temperature of 30 ℃ in a water bath shaker at 180r/min, and monitoring the complete degradation of organic matters through TOC, thus finishing the bacterial immobilization process. After the reaction is completed, slightly taking out the CuO NPs loaded PVA immobilized with the high-efficiency flora, slowly cleaning the PVA twice by MSM to remove free bacteria on the surface, adding the immobilized material loaded with bacteria into a coal chemical industry wastewater treatment system after pretreatment and biochemical treatment according to 12-15g of wastewater per liter for advanced treatment, and aerating and oxygenating for 12 hours to ensure that the COD of the effluent of the wastewater is 56mg/L, the ammonia nitrogen is reduced to 12mg/L, and the concentration of volatile phenol is 0.3 mg/L.
Example 2
Selecting the pretreated and biochemically treated wastewater generated by a certain coking enterprise as a research object to carry out a harmless advanced treatment field experiment, wherein the daily treated water amount of the wastewater treatment process of the enterprise is 3-5 tons, and the water quality of the field raw water, the pretreated and biochemically treated effluent is as follows:
TABLE 3 coking wastewater effluent quality of each stage
| Treatment stage | COD(mg/L) | Ammonia nitrogen (mg/L) | Volatile phenol (mg/L) |
| Raw water | 12500 | 1050 | 1150 |
| Physicochemical pretreatment | 3628 | 134 | 169 |
| A-O biochemistry | 152 | 12 | 17 |
Preparation of CuO NPs loaded PVA-based sponge carrier
Using PVA water-absorbing sponge as an immobilized carrier material, soaking and stirring the PVA-based sponge with 5% hydrochloric acid for 30min, washing the PVA-based sponge with pure water twice, soaking and stirring the PVA-based sponge with 5% sodium hydroxide for 30min, washing the PVA-based sponge with the pure water until the pH value is 7, soaking and ultrasonically treating the PVA-based sponge with the pure water for 1h, and drying the PVA-based sponge at 55 ℃. Adding the pretreated PVA-based sponge into a solution containing nano copper oxide at a ratio of 2.5g/L, fully mixing the mixed solution in an ultrasonic reactor for 30min, separating out the PVA-based sponge loaded with CuO NPs, drying at 60 ℃ for 12 h, and placing in a dry closed container for later use.
2. Culture of dominant flora of refractory organic matter
Expanded culture is carried out by adopting dominant flora after screening and domesticating in a laboratory, flora is inoculated firstly, culture is carried out for 24h in LB culture medium for enrichment, bacteria are added into an inorganic salt culture medium for domestication and immobilization after enrichment, and the concentration of the bacteria is controlled to OD600And (3) adding CuO NPs loaded PVA-based sponge material into the bacterial suspension according to the adding amount of 12-15g/L, simultaneously adding 100mg/L of quinoline, 100mg/L of phenol and 100mg/L of naphthalene as carbon sources, carrying out aerobic culture, keeping DO at 2.0-3.0mg/L, and monitoring the complete degradation of organic matters (TOC) by sampling to finish the bacterial immobilization process. After the reaction is completed, taking out the modified PVA material immobilized with the high-efficiency flora, adding the immobilized material loaded with bacteria into a coal chemical wastewater treatment system after biochemical treatment according to 12-15g of each liter of wastewater for advanced treatment, wherein the site temperature is 25-28 ℃, the pH of the wastewater is adjusted to about 7 by using diluted sodium hydroxide or hydrochloric acid, and after 12 hours of aeration and oxygenation, the COD of the effluent of the wastewater is reduced to 56mg/L, the ammonia nitrogen is reduced to 12mg/L, and the concentration of volatile phenol is 0.3 mg/L.
The preparation of the carrier and the process of flora domestication and immobilization are the same as the example 1, the adding amount of immobilized cells in the biochemical effluent is 15-20g per liter of wastewater, the COD of the effluent of the wastewater is reduced to 61mg/L, the ammonia nitrogen is reduced to 5mg/L, and the concentration of volatile phenol is 0.2mg/L after aeration oxygenation for 12 hours.
Claims (6)
1. A coal chemical industry wastewater advanced treatment method based on living cell immobilization technology is characterized by comprising the following steps:
step 1, performing physicochemical pretreatment and conventional biochemical treatment on coal chemical wastewater;
step 2, loading the domesticated dominant flora on a modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) based sponge carrier to prepare immobilized flora, and further adsorbing and metabolizing the organic matters which are difficult to degrade in the step 1 by using the obtained immobilized flora to realize harmless discharge of wastewater;
the preparation method of the modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) based sponge carrier comprises the following steps:
(1) pretreatment of PVA-based sponge: soaking and stirring the mixture for 20min to 30min by hydrochloric acid with the mass concentration of 5 percent to 8 percent, washing the mixture twice by pure water, soaking and stirring the mixture for 20min to 30min by sodium hydroxide with the mass concentration of 5 percent to 8 percent, washing the mixture by the pure water until the pH value is =6 to 8, soaking and ultrasonically treating the mixture for 1h to 2h by the pure water, and drying the mixture at the temperature of 50 ℃ to 60 ℃;
(2) preparing a modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) based sponge carrier: adding 0.2g-0.3g of pretreated PVA-based sponge into 80mL-150mL of nano copper oxide solution with the concentration of 50mg/L-150mg/L, fully mixing in an ultrasonic reactor for 30min-40min, separating out polyvinyl alcohol (PVA) -based sponge loaded with modified nano copper oxide CuO NPs, and carrying out vacuum drying at 50-60 ℃ for 10-15 hours to obtain the modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) -based sponge carrier;
the domestication method of the dominant flora comprises the following steps:
taking activated sludge as a bacteria source, adding tap water for dilution, carrying out aerobic culture at room temperature, standing, taking supernatant, inoculating the supernatant into a culture medium for culture and enrichment, cleaning bacteria by using sterilized inorganic salt after enrichment, simultaneously adding the bacteria into an inorganic salt culture medium for acclimatization culture, taking the organic matters which are difficult to degrade as a carbon source, inoculating and repeatedly acclimatizing, monitoring the condition of degrading the organic matters by the bacteria by taking TOC of a system as an index, and finally separating and purifying by adopting a plate scribing method to obtain a flora with a degradation effect meeting the requirement;
the process for preparing the immobilized flora comprises the following steps:
enriching the separated dominant flora by using a culture medium, cleaning by using inorganic salt to prepare a bacterial suspension, weighing a certain amount of modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) based sponge carrier, sterilizing, cooling to room temperature, adding the bacterial suspension into a reaction container, adding the organic matter which is difficult to degrade as a carbon source, carrying out aerobic culture, and monitoring the complete degradation of the organic matter by using TOC (total organic carbon), thereby completing the immobilization process of the flora;
and taking out the modified nano copper oxide CuO NPs-polyvinyl alcohol (PVA) based sponge carrier with immobilized flora, and slowly cleaning twice by using sterilized MSM to remove free bacteria on the surface for subsequent advanced treatment of the coal chemical industry wastewater.
2. The advanced treatment method for coal chemical industry wastewater based on the living cell immobilization technology as claimed in claim 1, wherein the mass ratio of the tap water to the activated sludge is 1:1, the aerobic culture time is 24 hours, the DO concentration is 2.0-3.0mg/L, the culture medium is LB culture medium, the culture is 24 hours, the dosage of the supernatant is 15mL, and the supernatant is inoculated in 85mL of sterilized culture medium for culture and enrichment.
3. The advanced treatment method for the coal chemical industry wastewater based on the living cell immobilization technology as claimed in claim 1, wherein the inorganic salt culture medium comprises the following components: na (Na)2HPO4 4.26 g/L，KH2PO4 2.65 g/L，MgSO4·7H2O 0.20 g/L，CaCl2 0.02 g/L，MnSO4·7H2O 0.002 g/L，(NH4)2SO40.4g/L and 1mL/L of trace elements, wherein the specific formula of the trace elements is as follows: FeCl2·4H2O 1.50 g/L, CuCl2·2H2O 0.002 g/L, MnSO4·7H2O 0.10 g/L, Na2MoO4·2H2O 0.024 g/L, ZnCl2 0.006 g/L, H3BO30.07g/L, adjusting pH of the culture medium to 7.0, sterilizing at 121 deg.C for 25min, and cooling.
4. The advanced treatment method for coal chemical industry wastewater based on living cell immobilization technology as claimed in claim 1, wherein the refractory organics are repeatedly acclimated in 15% inoculation amount, and the initial concentration of the refractory organics is 20 mg.L-1At 20 mg.L-1Gradually increased to a concentration of 200 mg/L.
5. The advanced treatment method for the coal chemical industry wastewater based on the living cell immobilization technology as claimed in claim 1, wherein the refractory organic matter is one or more of quinoline, phenol and naphthalene.
6. The advanced treatment method for coal chemical industry wastewater based on living cell immobilization technology as claimed in claim 1, wherein the inorganic salt is MSM, OD600And the solid-liquid ratio of the carrier to the bacterial suspension in the reaction vessel is 12-15g/L, the addition amount of the single refractory organic substance is 100mg/L, wherein the naphthalene is dissolved in acetone in advance.
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