CN103803755A - Processing method of waste water containing nitrophenol - Google Patents
Processing method of waste water containing nitrophenol Download PDFInfo
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- CN103803755A CN103803755A CN201210441772.XA CN201210441772A CN103803755A CN 103803755 A CN103803755 A CN 103803755A CN 201210441772 A CN201210441772 A CN 201210441772A CN 103803755 A CN103803755 A CN 103803755A
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Abstract
The invention provides a processing method of waste water containing nitrophenol, and belongs to the technical field of organic chemical industry waste water treatment. The processing method is specially used for processing nitrophenol compounds which are low in concentration, and are not needed to be recycled; CODCr removal rate of the waste water processed via the processing method is more than 85%, decolourization ratio is more than 95%, and the processed waste water is capable of meeting with national emission standards. The processing method comprises pretreatment of 4,6-diaminoresorcinol hydrochloride hydrolyzed waste water, and latter biochemical treatment; wherein according to the step of pretreatment, the hydrolyzed waste water is subjected to microelectrolysis, and then is subjected to catalytic oxidation. According to the processing method, in the step of pretreatment, the nitrophenol compounds which are difficult for biochemistry treatment are transformed into amines which are easy to oxidize, so that efficiency of subsequent biochemical treatment is increased greatly. Processing effects of the processing method are stable and reliable; processing cost is low; operation is simple and convenient; and industrialized application is easy to realize.
Description
Technical field
The present invention relates to the technical field of organic chemical waste water processing, furtherly, relate to the treatment process containing nitrophenol wastewater.
Background technology
4,6-diaminoresorcinol hydrochloride is the important source material of synthetic PBO, in production 4,6-diaminoresorcinol hydrochloride process, produces hydrolyzed waste water, contains nitrophenol compound in hydrolyzed waste water.Nitrophenol compound comprises mononitrophenol, dinitrophenol and picric acid.This compounds is all toxic to human body and mammals, is easily nitroso-group and azanol radical derivative by enzymatic conversion in vivo, and the former is carcinogens.Some nitrophenol toxicity are large and be difficult to biological degradation, can in environment, accumulate, and as 2-nitrophenol, 4-nitrophenol and 2,4-dinitrophenol.Treatment process for phenols wastewater mainly contains: Physical, and utilize physical action to remove pollutent in phenolic wastewater to reach the method for emission standard, mainly comprise solvent extration, absorption method and membrane separation process; Chemical oxidization method, industrial general employing Wet Catalytic Oxidation Method is processed at present.This method is to add catalyzer in traditional wet oxidation process, reduces the activation energy of reaction, thereby reaction can be completed under gentleer condition and in the shorter time.Study more oxygenant: Fenton reagent, hydrogen peroxide and dioxide peroxide etc.Biological process: the ultimate principle of biological treatment is the aldehydes matter utilizing in microorganism adsorption and Decomposition Wastewater, and objectionable impurities is changed into stable innoxious substance, its advantage is that equipment is simple, treatment effect good, the impact of climate condition is little etc.; Shortcoming is that pre-treatment requirement is high, and operation spending is larger.Apply more have activated sludge process, biological filter process, contact oxidation method and biological fluidized bed method.
Micro-electrolysis method is the more fruitful method of wastewater treatment growing up nineteen seventies.The 1980s, China started the research in this field, and make fast progress recent years.The biochemical Study on Oxidation of Organic of difficulty of the discharge such as current domestic mine industry, coking industry, petrochemical industry, organic chemical industry's compound probability, foodstuffs industry, leather industry, pharmaceutical industry and printing and dyeing industry is more.
Su Ying, Dan Mingjun etc., take the beautiful powdered graphite of steel scrap and waste iron filing as electrode, adopt short distance digestion-micro-electrolysis process to carry out denitrogenation processing to coking chemical waste water.Result shows: the micro-electrolysis process NO of short distance nitration-iron charcoal
2the clearance of-N is 57.0%.The clearance of TN is 50.0%.
Appoint rosy clouds, Liu Li etc. adopt micro-electrolysis-UASB-bio-contact oxidation tandem process to process the high density organic acidity waste water that oil product synthesizing section produces.Result shows: micro-electrolysis pretreatment effectively reduces waste water acidity and CODcr,, for condition has been created in follow-up biochemical treatment.
See from the present Research of the micro-electrolysis of current iron charcoal, iron charcoal micro electrolysis tech carrying out thering is less investment in sewage preprocessing process, working cost is low, simple operation and other advantages, especially very large in the effect of processing the performance of difficult biochemical aromatic series organic pollutant field.
The hydrolyzed waste water producing in 4,6-diaminoresorcinol hydrochloride process, is that a kind of phenol content is lower, does not possess the directly biochemical waste water that is difficult to of recovery value.Therefore adopt the micro-electrolysis of iron charcoal, in conjunction with ClO 2 catalyzed oxidation method, waste water is carried out to pre-treatment, difficult biochemical nitrophenol compound is converted into oxidizable amine, thereby can greatly improves the efficiency of follow-up biochemical treatment.
Summary of the invention
The object of the invention is for proposing a kind for the treatment of process containing nitrophenol wastewater.Described is to produce 4 containing nitrophenol wastewater, in 6-diamino resorcin hydrochlorate process, the waste water producing when hydrolysis, in this waste water, feature pollutent is chloro-(4, the 6)-dinitroresorcinol of 2-, before processing, COD is greater than 10000mg/L, after pre-treatment of the present invention, CODCr clearance can reach more than 65%, is conducive to follow-up biochemical treatment.Final CODCr can, lower than below 800mg/L, reach discharging standards.
Main technical schemes of the present invention: first to Wastewater Pretreatment, carry out afterwards biochemical treatment.Described pre-treatment comprises carries out microelectrolysis processing and two steps of catalytic oxidation treatment to 4,6-diaminoresorcinol hydrochloride hydrolyzed waste water, and described biochemical treatment is the activated sludge biochemical processing that this area adopts conventionally.
Concrete steps are as follows: regulating waste water ph is 1-2, adds iron powder, powdered carbon, and it definitely adds ratio at 2:1, control iron powder and the total amount of powdered carbon and the ratio of waste water total amount and are not less than 0.03; After controlling in iron charcoal input water, the residence time is 5-6 hours;
Regulate waste water ph to 5-6, passed into overflow type fixed bed catalytic oxidation tower, add Chlorine Dioxide Oxidation agent, control Chlorine Dioxide Oxidation agent add-on and be not less than 0.25 with the relative volume ratio of wastewater flow rate, the residence time that control waste water enters catalyzed oxidation tower is 50-60 minutes, in raw wastewater, nitro-phenolic compound has been oxidized to the amido thing of easy biochemistry, directly enters biochemical.
For iron charcoal microelectrolysis process, pH is very large on iron charcoal treatment effect impact, and the transformation efficiency of the less nitrophenol of pH is higher, when main because pH value is lower, and a large amount of H in solution
+, accelerated microbattery reaction process and Fe
2+stripping, strengthened the Degradation of its p-nitrophenol.But neither pH value the smaller the better, when pH value is very low, need to consume the acid in a large amount of preprocessing process, increase the consumption of Fe, also higher to the requirement of processing vessel, these all can increase processing cost; The too much Fe that reaction produces on the other hand
2+can make chroma in waste water after treatment high, and produce a large amount of iron mud, increase the weight of processing load.In this process, pH 1-2 is top condition.
For iron charcoal microelectrolysis process, the degraded of iron powder amount p-nitrophenol has a certain impact, and when Fe measures when little, does not have enough Fe and C to form galvanic cell, so the transformation efficiency of nitrophenol is very low in solution.And along with the increase of iron powder consumption, the transformation efficiency of nitrophenol increases, but when iron filings consumption reaches certain value, transformation efficiency is comparatively stable, illustrates that Fe measures enough to have maintained reaction.Therefore control iron powder, the absolute ratio of powdered carbon is 2:1, the ratio of the total amount of iron powder, powdered carbon and waste water total amount is more than or equal to 0.03.
For iron charcoal microelectrolysis process, because iron charcoal is the effect of micro-electrolysis, the conversion rate of nitrophenol is very fast, the microbattery forming due to iron charcoal and the adsorption of iron filings, and the transformation efficiency of nitrophenol also keeps higher level.But along with the prolongation in reaction times, iron filings surface is because of oxidation or the attached collection of pollutent precipitates passivation gradually, and the concentration of nitrophenol is very low in the situation that, and speed of reaction is very slow, until balance.In this process, regulate most optimal retention time 5-6 hours.
For ClO 2 catalyzed oxidation process, wastewater pH is pulled back to 5-6, because pH not only can affect ClO
2redox potential, also can change amine and have a form in water, be therefore the important factor that affects speed of reaction.Under solutions of weak acidity, charcoal absorption effect is strong, organism in energy active adsorption waste water, thereby speed of reaction is fast, is conducive to water treatment.General by adding 20% NaOH solution to regulate pH.
For ClO 2 catalyzed oxidation process, be difficult to or not oxidized organism owing to containing some in waste water, these organism occur isolated poisoning in the enrichment meeting of catalyst surface, reduce the catalytic performance of catalyzer, thereby organic clearance in reduction waste water, the reduction of clearance affects again the work-ing life of catalyzer, increases processing cost, so consider to add strong oxidizer dioxide peroxide to destroy the structure of these difficult oxidation of organic compounds, improve the work-ing life of catalyzer.Considering to add dioxide peroxide is because dioxide peroxide can rapid and most of organism generation oxidizing reaction.The consumption of oxygenant is relevant with the concentration of difficult oxidizing substance in waste water, the increase of oxygenant consumption can improve oxidation efficiency, but can increase substantially processing cost, for 4,6-diamino resorcin hydrochlorate hydrolyzed waste water, Chlorine Dioxide Oxidation agent add-on is not less than 0.25 with the relative volume ratio of wastewater flow rate.
For ClO 2 catalyzed oxidation process, the prolongation of oxidization time will improve organic oxidation depth, and small organic molecule will continue to be oxidized to CO
2and water, directly show that COD clearance will increase.In general, oxidizing reaction is after certain hour, and COD clearance will increase slowly.The increase of the oxidation residence time can improve COD clearance, but can increase the investment of equipment, and for 4,6-diaminoresorcinol hydrochloride hydrolyzed waste water, waste water enters catalyzed oxidation tower by upper inlet, overflow type water outlet, and the residence time is 50-60 minutes.
The treatment process of 4,6-diaminoresorcinol hydrochloride hydrolyzed waste water of the present invention, catalyzed oxidation adopts the mode of continuous effluent, and catalyzed oxidation tower is selected overflow type fixed bed.
The invention provides a kind of for 4,6-diamino resorcin hydrochlorate hydrolyzed waste water, is converted into amine through the pre-treatment of the micro-catalytic and oxidative electrolysis technology of iron charcoal by nitro-compound in waste water, reduces the toxicity in sewage, improve the biodegradability of sewage, finally by biochemical treatment rear discharge up to standard simultaneously.Waste water COD after treatment
crclearance can reach more than 85%, and percent of decolourization can reach more than 95%.
Compared with prior art, the present invention has following advantage:
1) relatively test stability high, high for the clearance of nitro-phenolic compound in waste water.
2) relative good decolorizing effect.COD clearance is higher.
3) process of the test is simple relatively, and cost is lower, is applicable to industrialization operation.
Embodiment
Below in conjunction with embodiment, treatment process of the present invention is described in detail.
Embodiment 1
Get 600ml4,6-diamino resorcin hydrochlorate hydrolyzed waste water, COD11674mg/L after filtering, regulates its pH in 1 backward reactor, to add 20g iron powder and 10g active carbon powder, under the condition stirring, reacts 6 hours, afterwards the wastewater pH after micro-iron charcoal electrolysis is pulled back to 5, after mixing with 200ml Chlorine Dioxide Oxidation agent solution again, enter oxide pillars by oxide pillars top, the air feed of intaking continuously, overflow water outlet, regulate volume pump, being controlled at the residence time is 80 minutes.After 8 hours, sample water outlet COD1944mg/L after micro-catalytic and oxidative electrolysis technology, colourity is less than 50.After activated sludge biochemical is processed afterwards, COD678 mg/L, and biochemical reaction operational excellence.
Embodiment 2
Get 600ml4,6-diamino resorcin hydrochlorate hydrolyzed waste water, COD12474mg/L after filtering, regulates its pH in 1 backward reactor, to add 16g iron powder and 8g active carbon powder, under the condition stirring, reacts 6 hours, afterwards the wastewater pH after micro-iron charcoal electrolysis is pulled back to 6, after mixing with 300ml Chlorine Dioxide Oxidation agent solution again, enter oxide pillars by oxide pillars top, the air feed of intaking continuously, overflow water outlet, regulate volume pump, being controlled at the residence time is 60 minutes.After 16 hours, sample water outlet COD1746mg/L after micro-catalytic and oxidative electrolysis technology, colourity is less than 50.After activated sludge biochemical is processed afterwards, COD658mg/L, and biochemical reaction operational excellence.
Embodiment 3
Get 600ml4,6-diamino resorcin hydrochlorate hydrolyzed waste water, COD11189mg/L after filtering, regulate its pH in 1 backward reactor, to add 16g iron powder and 8g active carbon powder, under the condition stirring, react 6 hours, afterwards the wastewater pH after micro-iron charcoal electrolysis is pulled back to 6, after mixing with 300ml Chlorine Dioxide Oxidation agent solution again, together add loading catalyst graduated cylinder, aeration is provided, the oxidation of employing intermittent type, react liquid Analysis for CO D 1890 mg/L in taken amount cylinder upper strata after 80 minutes, colourity is less than 50.After activated sludge biochemical is processed afterwards, COD895mg/L, and biochemical reaction operational excellence.This embodiment can find out that intermittent type oxidation unit is also feasible, but considers in suitability for industrialized production, and need continuous influent, therefore the present invention selects continous way catalytic oxidizing equipment more.
Embodiment 4
Get 600ml4,6-diamino resorcin hydrochlorate hydrolyzed waste water, COD12451mg/L after filtering, regulates its pH in 1 backward reactor, to add 16g iron powder and 8g active carbon powder, under the condition stirring, reacts 6 hours, afterwards the wastewater pH after micro-iron charcoal electrolysis is pulled back to 6, after mixing with 300ml Chlorine Dioxide Oxidation agent solution again, enter oxide pillars by oxide pillars top, the air feed of intaking continuously, overflow water outlet, regulate volume pump, being controlled at the residence time is 60 minutes.After 4 hours, sample water outlet COD3235mg/L after micro-catalytic and oxidative electrolysis technology, colourity is less than 50.This embodiment can find out, in long run test, steady time is too short, and water outlet COD does not reach optimum handling effect.
Claims (9)
1. containing the treatment process of nitrophenol wastewater, it is characterized in that first, to Wastewater Pretreatment, carrying out afterwards biochemical treatment, described pre-treatment comprises carrying out microelectrolysis processing and two steps of catalytic oxidation treatment containing nitrophenol wastewater:
Adjusting waste water ph is 1-4, adds iron powder, powdered carbon, and it adds ratio at 2:1, and the ratio of the total amount of iron powder and powdered carbon and waste water total amount is not less than 0.03; After iron charcoal drops in water, the residence time is 4-8 hour;
Regulate waste water ph to 4-7, passed into overflow type fixed bed catalytic oxidation tower, add Chlorine Dioxide Oxidation agent, Chlorine Dioxide Oxidation agent add-on is not less than 0.25 with the relative volume ratio of wastewater flow rate, and the residence time that waste water enters catalyzed oxidation tower is 30-80 minute.
2. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, reconciles its pH value for 1-2.
3. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, control iron powder, the absolute ratio of powdered carbon are 2:1, the ratio of the total amount of iron powder, powdered carbon and waste water total amount is more than or equal to 0.03.
4. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, after iron charcoal drops in water, the residence time is 5-6 hour.
5. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, before adding Chlorine Dioxide Oxidation agent, is adjusted to 5-6 by waste water ph.
6. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, controls Chlorine Dioxide Oxidation agent add-on and is not less than 0.25 with the relative volume ratio of wastewater flow rate.
7. treatment process according to claim 1, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, the residence time that waste water enters catalyzed oxidation tower is 50-60 minute.
8. according to the treatment process described in claim 1 or 7, while it is characterized in that waste water to carry out micro-catalytic and oxidative electrolysis technology processing, catalyzed oxidation tower is selected overflow type fixed bed.
9. treatment process according to claim 1, is characterized in that catalyzed oxidation adopts the mode of continuous effluent.
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Cited By (3)
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| CN104355465A (en) * | 2014-10-31 | 2015-02-18 | 江苏南大环保科技有限公司 | Method for eliminating tar in micro-electrolysis reduction denitration process |
| CN106315965A (en) * | 2015-06-23 | 2017-01-11 | 中国石油化工股份有限公司 | Treatment method of wastewater in 4,6-dinitro-1,2,3-trichlorobenzene hydrolysis reaction |
| CN107188296A (en) * | 2017-07-28 | 2017-09-22 | 辽东学院 | The method that chlorine dioxide mixed oxidization method handles amino phenols waste water from dyestuff |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355465A (en) * | 2014-10-31 | 2015-02-18 | 江苏南大环保科技有限公司 | Method for eliminating tar in micro-electrolysis reduction denitration process |
| CN104355465B (en) * | 2014-10-31 | 2016-03-16 | 江苏南大环保科技有限公司 | The method of the coal-tar middle oil releasing of a kind of light electrolysis reduction denitrification process |
| CN106315965A (en) * | 2015-06-23 | 2017-01-11 | 中国石油化工股份有限公司 | Treatment method of wastewater in 4,6-dinitro-1,2,3-trichlorobenzene hydrolysis reaction |
| CN107188296A (en) * | 2017-07-28 | 2017-09-22 | 辽东学院 | The method that chlorine dioxide mixed oxidization method handles amino phenols waste water from dyestuff |
| CN107188296B (en) * | 2017-07-28 | 2020-08-18 | 辽东学院 | Method for treating aminophenol dye wastewater by chlorine dioxide mixed oxidation method |
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Application publication date: 20140521 |